CN102419357B - Method for detecting eighteen-component codonopsis pilosula preparation - Google Patents

Method for detecting eighteen-component codonopsis pilosula preparation Download PDF

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CN102419357B
CN102419357B CN201110443891.4A CN201110443891A CN102419357B CN 102419357 B CN102419357 B CN 102419357B CN 201110443891 A CN201110443891 A CN 201110443891A CN 102419357 B CN102419357 B CN 102419357B
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CN102419357A (en
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陈丽娟
张国霞
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Tibet Cheezheng Tibetan Medicine Co Ltd
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Tibet Cheezheng Tibetan Medicine Co Ltd
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Abstract

The invention relates to a detecting method for an eighteen-component codonopsis pilosula preparation, which comprises one or more of the following identification and/or detection methods: identifying the morphological characteristics of medical materials such as Tibetan codonopsis pilosula, Bangna (a traditional Chinese medicament), cassia seed, Tibetan drug sweetflag rhizome, Chinese tinospora stem, denucleated medicament terminalia fruit, gymnadenia conopsea, fructus terminaliae billericae, frankincense, Kukuinabu (a traditional Chinese medicament) and Baxiaga (a Traditional Tibetan medicament containing vasicine) in the preparation through a microscope; qualitatively identifying costustoot, the Tibetan drug sweetflag rhizome and the frankincense in the preparation through thin layer chromatography; and detecting the content of aconitine in the preparation. By the method, the eighteen-component codonopsis pilosula preparation can be effectively detected.

Description

The detection method of 18 taste asiabell preparations
Technical field
The invention belongs to technical field of traditional Chinese medicines, be specifically related to a kind of detection method of Chinese medicine preparation.
Background technology
18 taste Radix Codonopsis balls are Tibetan medicine's tradition proved recipes, prescription by ZANGDANGSHEN, list that, cassia seed, Dong Siba, slag tame and docile cream, BAXIAGA, emblic and the banksia rose 18 taste medicinal materials such as cream, Rhizoma Acori Calami, wide muscle rattan, myrobalan, hand ginseng, terminaliae billericae,fructus, Moschus, frankincense, Semen seu folium abelmoschi moschati, bitter Kui Nabu, Song Sheng and form, there is anti-inflammatory analgetic, more sore, except effect of yellow water.For numbness disease, " ridge bar " disease, extremities joint congestion and swelling pain, it is in the wrong unfavorable to stretch, eczema, psoriasis, falls into erosion tinea, pestilence pain, sub-agate parasitosis and leprosy.
The quality inspection standard of the 18 taste Radix Codonopsis balls that use is at present recorded in first of Ministry of Public Health's Tibetan medicine standard:
18 taste Radix Codonopsis balls, phonetic name: Shibawei Dangsheng Wan
Book page number: C1-189 standard number: WS3-BC-0186-95
[prescription] 150g of ZANGDANGSHEN, tendril-leaved fritillary bulb 300g, cassia seed 80g, high mountain corydalis 10g, slag are tamed and dociled cream 10g, Rhizoma Acori Calami 40g, wide muscle rattan 70g, myrobalan 50g, hand ginseng 7.5g, terminaliae billericae,fructus 8.5g, Moschus 5g, frankincense 70g, Semen seu folium abelmoschi moschati 70g, styrax 50g, catechu 70g, BAXIAGA 70g, emblic 70g, banksia rose 75g.
[method for making] above 18 tastes, tame and docile the another porphyrize powder of cream except Moschus, slag, and all the other are ground into fine powder altogether, sieve, and add Moschus fine powder, mix, and tame and docile cream add appropriate water pill with slag, dry in the shade, and to obtain final product.
[proterties] this product is the yellow water-bindered pill; The micro-perfume (or spice) of gas, bitter.
[discriminating] got this product and put micro-Microscopic observation: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell.Amylum body, simple grain circle triangle, similar round, omphalion is obvious, herringbone shape, horse-hof shape, crosswise, diameter 4～35 μ m; How in blocks seed coat palisade cells is, colourless or faint yellow, and surface is seen and is class polygon, the micro-shrinkage of wall; Pollen granule class spheroidal, the visible sparse circular boss in surface, diameter 35 μ m, 3 of germinal furrows; The normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, diameter 6～20 μ m, end is point gradually, lignify.Pericyclic fiber is slightly thick, and pit is obvious, and diameter 10～13 μ m are normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber.In groups, some summary branches or one end slightly point are prominent for lithocyte, wall thickness 8～20 μ m, and hole ditch is fine and closely woven and clear.Needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in, long 8～65 μ m; Endocarp is the prothenchyma (of wood) extending, long 25～180 μ m, diameter 18～28 μ m, wall thickness, lignify; Faint yellow agglomerate is by assembling and form containing granular substance square, cylindricality crystallization; Conduit is bordered pit, diameter 40～110 μ m; Resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious.The block of raphides and yellowish-brown is numerous; Mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal, diameter 48～60 μ m.Leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.Synanthrin is common, fan-shaped, the existing radial texture in surface.
[inspection] should meet every regulation relevant under pill item (8 pages of annex).
[function with cure mainly] anti-inflammatory analgetic, more sore, except yellow water.For numbness disease, " ridge bar " disease, extremities joint congestion and swelling pain, it is in the wrong unfavorable to stretch, eczema, psoriasis, falls into erosion tinea, pestilence pain, sub-agate parasitosis and leprosy.
[usage and consumption] 3 balls, 3 times on the one.
The heavy 1g of [specification] every ball.
[storage] is airtight, puts shady and cool dry place.
Current quality inspection standard only uses microscope to differentiate, specificity and the reappearance of this detection method are further improved, in addition this detection method do not comprise to prescription in toxic component carry out limit examine.
Summary of the invention
The object of the present invention is to provide a kind of detection method of 18 taste asiabell preparations.
For achieving the above object, technical scheme of the present invention is:
A kind of detection method of 18 taste asiabell preparations, said preparation bulk drug consists of: the 120-240 of ZANGDANGSHEN weight portion, that 80-320 weight portion of tendril-leaved fritillary bulb/list, cassia seed 50-120 weight portion, high mountain corydalis/Dong Siba 5-120 weight portion, slag is tamed and dociled cream 5-80 weight portion, Rhizoma Acori Calami 20-180 weight portion, wide muscle rattan 50-120 weight portion, the myrobalan 25-180 weight portion of stoning, hand ginseng 1-120 weight portion, terminaliae billericae,fructus 1-120 weight portion, Moschus/muscone 0.1-10 weight portion, frankincense 50-120 weight portion, Semen seu folium abelmoschi moschati 50-100 weight portion, styrax/bitter Kui Nabu 30-120 weight portion, the cream 30-100 weight portions such as catechu/Song Sheng, BAXIAGA 50-120 weight portion, emblic 50-120 weight portion, banksia rose 50-120 weight portion,
The method comprises one or more of following discriminating and/or inspection method:
By microscope differentiate preparation Chinese crude drug ZANGDANGSHEN, list that, the morphological feature of cassia seed, Rhizoma Acori Calami, wide muscle rattan, myrobalan, hand ginseng, terminaliae billericae,fructus, frankincense, bitter Kui Nabu, BAXIAGA;
By thin-layer chromatography, the banksia rose in preparation, Rhizoma Acori Calami, frankincense are carried out to qualitative discriminating, and check preparation mesaconitine content.
Particularly, described microscope is differentiated and is comprised the steps:
Get described 18 taste asiabell preparations and put micro-Microscopic observation, differentiate the morphological feature of following ingredients, wherein:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells;
The qualitative discriminating of the banksia rose comprises:
1a) prepare the negative sample solution that the banksia rose is determined need testing solution, banksia rose control medicinal material solution, do not contained the banksia rose;
2a), according to 2010 editions one annex VI B of thin-layered chromatography " Chinese Pharmacopoeia " test, draw respectively step 1a) need testing solution, control medicinal material solution, the negative sample solution that obtain, and point sample is on same silica gel g thin-layer plate;
3a) taking cyclohexane-methylene chloride-ethyl acetate as developping agent, by step 2a) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, spray is with vanillic aldehyde sulfuric acid solution, wind is clear to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
The qualitative discriminating of Rhizoma Acori Calami comprises:
1b) prepare the need testing solution, Rhizoma Acori Calami control medicinal material solution of Rhizoma Acori Calami, not containing the negative sample solution of Rhizoma Acori Calami;
2b), according to 2010 editions one annex VI B of thin-layered chromatography " Chinese Pharmacopoeia " test, draw respectively step 1b) need testing solution, control medicinal material solution, the negative sample solution that obtain, and point sample is on same silica gel g thin-layer plate;
3b) taking petroleum ether-ethyl acetate as developping agent, by step 2b) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out,, dry, put under ultraviolet lamp and inspect; In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
The qualitative discriminating of frankincense comprises:
1c) prepare the need testing solution, frankincense control medicinal material solution of frankincense, not containing the negative sample solution of frankincense;
2c), according to 2010 editions one annex VI B of thin-layered chromatography " Chinese Pharmacopoeia " test, draw respectively step 1c) need testing solution, control medicinal material solution, the negative sample solution that obtain, and point sample is on same silica gel g thin-layer plate;
3c) taking cyclohexane-ethyl acetate as developping agent, by step 2c) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, wind is clear to spot colour developing; In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
Content of Aconitine inspection comprises:
1d) prepare need testing solution, the aconitine control medicinal material solution of aconitine;
2d), according to annex VI B test of thin-layered chromatography " Chinese Pharmacopoeia " version in 2010, draw respectively step 1d) need testing solution, the aconitine control medicinal material solution that obtain, and point sample is on same silica gel g thin-layer plate;
3d) taking toluene-ethyl acetate-diethylamine as developping agent, by step 2d) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, spray is with rare bismuth potassium iodide test solution; In thin-layer chromatography, test sample chromatogram with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The preparation method of the need testing solution of the described banksia rose, Rhizoma Acori Calami, frankincense and aconitine, control medicinal material solution, negative sample solution comprises:
(1) need testing solution of the banksia rose, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, porphyrize, adds methyl alcohol, and ultrasonic processing filters, and filtrate is concentrated, as the need testing solution of the banksia rose; Separately get dehydro-α-curcumene control medicinal material, be made in the same way of banksia rose control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution;
(2) need testing solution of Rhizoma Acori Calami, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, porphyrize, adds diethyl ether, and ultrasonic processing filters, and filtrate volatilizes, and residue adds diethyl ether and makes to dissolve, as the need testing solution of Rhizoma Acori Calami; Separately get Rhizoma Acori Calami control medicinal material, be made in the same way of Rhizoma Acori Calami control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution;
(3) need testing solution of frankincense, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, porphyrize, adds acetone, and ultrasonic processing filters, and filtrate is concentrated into, as the need testing solution of frankincense; Separately get frankincense control medicinal material, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.
(4) need testing solution of aconitine, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, put in tool plug conical flask, add diethyl ether, ammonia solution, close plug, shake up, place, filter, the dregs of a decoction add diethyl ether, jolting, filter, the dregs of a decoction wash with ether again, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride to be made to dissolve, be transferred in separating funnel, with methenyl choloride gradation washing container, washing lotion is incorporated in separating funnel, extract with 0.05mol/L sulfuric acid solution, merge acid solution, add ammonia solution and regulate pH value extremely, extract with methenyl choloride again, merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol to be made to dissolve, as the need testing solution of aconitine, separately get aconitine control medicinal material, add absolute ethyl alcohol and make control medicinal material solution.
Preferably, said method comprising the steps of:
A) the qualitative discriminating of the banksia rose
Get described 18 taste asiabell preparation 0.5～2 weight portions, porphyrize, adds methyl alcohol 5～20 parts by volume, and ultrasonic processing 20～45 minutes filters, and filtrate is concentrated into 1～3 parts by volume, as the need testing solution of the banksia rose; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every parts by volume containing 0.0005 weight portion; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw each 0.003～0.007 parts by volume of above-mentioned three kinds of solution, point sample is on same silica gel g thin-layer plate respectively, and with cyclohexane-methylene chloride-ethyl acetate, volume ratio is 10～20: 2～8: 0.5～2 is developping agent, thin layer plate is put in expansion cylinder saturated 0～40 minute, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
B) the qualitative discriminating of Rhizoma Acori Calami
Get described 18 taste asiabell preparation 1～5 weight portions, porphyrize, 5～20 parts by volume that add diethyl ether, close plug, shakes up, ultrasonic processing 20～45 minutes, filter, filtrate volatilizes, residue add diethyl ether 1～3 parts by volume make dissolve, as the need testing solution of Rhizoma Acori Calami; Separately get Rhizoma Acori Calami control medicinal material 0.1～0.8 weight portion, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw each 0.005～0.02 parts by volume of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as 60 DEG C～90 DEG C petroleum ether-ethyl acetates are as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=2～8: 0.5～2, thin layer plate is put in expansion cylinder saturated 0～40 minute, launches, and takes out, dry, put under 254nm ultraviolet lamp and inspect; In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
C) the qualitative discriminating of frankincense
Get described 18 taste asiabell preparation 0.5～3 weight portions, porphyrize, adds acetone 5～20 parts by volume, and ultrasonic processing 20～45 minutes filters, and filtrate is concentrated into 1～3 parts by volume, as the need testing solution of frankincense; Separately get frankincense control medicinal material 0.1～0.8 weight portion, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 0.003～0.007 parts by volume, negative sample solution 0.003～0.007 parts by volume, control medicinal material solution 0.001～0.003 parts by volume, put respectively on same silica gel g thin-layer plate, taking volume ratio as 5～15: cyclohexane-ethyl acetate of 0.5～2 is developping agent, thin layer plate is put in expansion cylinder saturated 0～40 minute, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
D) the content inspection of aconitine
Get described 18 taste asiabell preparation 2～8 weight portions, put in tool plug conical flask, 15～40 parts by volume add diethyl ether, ammonia solution 1～5 parts by volume, close plug, shake up, place 18～30 hours, filter, the dregs of a decoction 30～70 parts by volume that add diethyl ether, jolting 0.5～2 hour, filter, the dregs of a decoction are again with ether washing 1～3 time, each 5～25 parts by volume, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 5～20 parts by volume to be made to dissolve, be transferred in separating funnel, with methenyl choloride 5～20 parts by volume gradation washing containers, washing lotion is incorporated in separating funnel, with 0.05mol/L sulfuric acid solution extraction 2～6 times, merge acid solution, add ammonia solution and regulate pH value to 7～11, extract 2～5 times with methenyl choloride again, merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1～3 parts by volume to be made to dissolve, as the need testing solution of aconitine, it is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every parts by volume containing 0.0005～0.002 weight portion, medicinal material solution in contrast, according to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, accurate need testing solution 0.003～0.007 parts by volume, control medicinal material solution 0.003～0.007 parts by volume drawn, put respectively on same silica gel g thin-layer plate, taking volume ratio as 10～20: 2～6: toluene-ethyl acetate-diethylamine of 0.5～2 is developping agent, thin layer plate is put in expansion cylinder saturated 0～40 minute, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
More preferably, said method comprising the steps of:
I) the qualitative discriminating of the banksia rose:
Get described 18 taste asiabell preparation 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as the need testing solution of the banksia rose; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 15: 5: 1 developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
Ii) the qualitative discriminating of Rhizoma Acori Calami:
Get described 18 taste asiabell preparation 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5: 1, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
Iii) the qualitative discriminating of frankincense
Get described 18 taste asiabell preparation 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 9: 1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
Iv) the content inspection of aconitine
Get described 18 taste asiabell preparation 5g, put in tool plug conical flask, 25mL adds diethyl ether, ammonia solution 3mL, close plug, shake up, place 24 hours, filter, the dregs of a decoction 50mL that adds diethyl ether, jolting 1 hour, filter, the dregs of a decoction are again with ether washing 2 times, each 15mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 10mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 10mL gradation washing container, washing lotion is incorporated in separating funnel, with 0.05mol/L sulfuric acid solution extraction 4 times, merge acid solution, add ammonia solution and regulate pH value to 9, extract 3 times with methenyl choloride again, merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 2mL to be made to dissolve, as need testing solution, it is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1mg, medicinal material solution in contrast, according to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, accurate need testing solution 5 μ L, the control medicinal material solution 5 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking volume ratio as the toluene-ethyl acetate-diethylamine of 14: 4: 1 is as developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The formulation of above-mentioned 18 taste asiabell preparations can be tablet, capsule, granule, pill or powder.Preparation method is: get described 18 taste asiabell preparations, be ground into fine powder, sieve, mix, add suitable quantity of water pill, dry in the shade and get final product; Or get described 18 taste asiabell preparations, and be ground into fine powder, sieve, mix, by pharmacy conventional method, add conventional auxiliary material, make the oral formulations of accepting clinically.
The present invention is directed to the constituent of 18 taste asiabell preparations, the existence of the index composition banksia rose, frankincense, Rhizoma Acori Calami is detected, and detect the content of the toxic component aconitine in preparation, to reach the object that the quality of preparation is controlled.Detection method of the present invention detects needs according to reality, and the testing conditions of existing detection method is screened, and has determined the preferably detection method of 18 taste asiabell preparations, and that this detection method has is sensitive, favorable reproducibility and the strong feature of specificity.
Brief description of the drawings
Fig. 1 is the micro-discriminating figure of 18 taste asiabell preparation;
Fig. 2 is banksia rose thin-layer chromatography discriminating figure in 18 taste asiabell preparations;
Wherein sample order is from left to right: need testing solution 1, need testing solution 2, need testing solution 3, dehydro-α-curcumene control medicinal material solution, dehydro-α-curcumene control medicinal material solution, banksia rose negative controls;
Wherein developping agent is cyclohexane-methylene chloride-ethyl acetate (15: 5: 1).
Fig. 3 is Rhizoma Acori Calami thin-layer chromatography discriminating figure in 18 taste asiabell preparations;
Wherein sample order is from left to right: need testing solution 1, need testing solution 2, need testing solution 3, Rhizoma Acori Calami control medicinal material solution, Rhizoma Acori Calami control medicinal material solution, Rhizoma Acori Calami negative controls;
Wherein developping agent is sherwood oil (60 DEG C～90 DEG C)-ethyl acetate (5: 1).
Fig. 4 is frankincense thin-layer chromatography discriminating figure in 18 taste asiabell preparations;
Wherein sample order is from left to right: need testing solution 1, need testing solution 2, need testing solution 3, frankincense control medicinal material solution, frankincense control medicinal material solution, frankincense negative controls;
Wherein developping agent is cyclohexane-ethyl acetate (9: 1).
Fig. 5 is the thin-layer chromatogram that 18 taste asiabell preparation mesaconitine content check;
Wherein sample order is from left to right: need testing solution 1, need testing solution 2, need testing solution 3, aconitine control medicinal material solution, aconitine control medicinal material solution, that negative controls of list;
Wherein developping agent is toluene-ethyl acetate-diethylamine (14: 4: 1).
Embodiment
Following experimental example and embodiment further illustrate but are not limited to the present invention.
The following preparation of differentiating for each composition under each discrimination method all referred to as " test sample ", being interpreted as it and referring to the test sample of preparing according to each discrimination method requirement, for example, is " test sample of the qualitative discriminating of the banksia rose " at the test sample described in the qualitative discrimination method of the banksia rose.
Experimental example 1: micro-discriminating
Get described 18 taste Radix Codonopsis honeyed bolus, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
Have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell.Synanthrin is fan-shaped, the existing radial texture (ZANGDANGSHEN) in surface.Amylum body is numerous, and simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, and omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain (list that).How in blocks seed coat palisade cells is, colourless or faint yellow, and surface is seen and is class polygon, the micro-shrinkage of wall (cassia seed).The normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point (Rhizoma Acori Calami) gradually.Pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, forms crystal fiber (wide muscle rattan).Lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round includes calcium oxalate cluster crystal (myrobalan).Needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in (hand ginseng).Nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing (terminaliae billericae,fructus).Irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve (frankincense).Resin crystallization is unsetting, and rufous is translucent, and corner angle are (bitter Kui Nabu) obviously.Leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells (BAXIAGA).The results are shown in Figure 1.
Experimental example 2: the thin layer of the banksia rose is differentiated
(1) instrument
Mortar, electronic scales, tool plug conical flask, transfer pipet, ultrasound wave extraction apparatus, funnel, filter paper, evaporating dish, sample applicator, silica gel g thin-layer plate, double flute chromatography cylinder, spray bottle, hair dryer.
(2) control medicinal material
Dehydro-α-curcumene control medicinal material (lot number: 111525-200907), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
(3) reagent
Methyl alcohol, acetone, cyclohexane, methylene chloride, ethyl acetate, 5% vanillic aldehyde sulfuric acid solution.
(4) method of inspection:
Extract the selection of solvent: adopt respectively methyl alcohol and acetone for extracting solvent;
The selection of extracting method: adopt respectively ultrasonic processing and add hot reflux;
The selection of developping agent: cyclohexane-methylene chloride-ethyl acetate (15: 5: 1), cyclohexane-ethyl acetate (9: 1) are developping agent respectively.
(5) select respectively above different solvents, extracting method and developping agent to test, result is as follows:
Repetition test in the above conditions, finally determine that the specificity thin-layer identification method of the banksia rose is as follows:
Get described 18 taste asiabell preparation 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 15: 5: 1 developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose reference substance chromatogram on, the spot of the aobvious same color of test sample chromatogram.As shown in Figure 2.The method operates through many people test of many times, favorable reproducibility, and specificity is strong, can be used as the detection method of 18 taste asiabell preparations.
Experimental example 3: the thin layer of Rhizoma Acori Calami is differentiated
(1) instrument
Mortar, electronic scales, tool plug conical flask, transfer pipet, ultrasound wave extraction apparatus, funnel, filter paper, evaporating dish, sample applicator, silica G F 254plate, chromatography cylinder, ultraviolet point sample analyser.
(2) control medicinal material
Rhizoma Acori Calami control medicinal material (lot number: 121084-200502), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
(3) reagent
Methyl alcohol, ether, sherwood oil (60 DEG C～90 DEG C), ethyl acetate, formic acid.
(4) method of inspection:
Extract the selection of solvent: adopt respectively methyl alcohol and ether for extracting solvent;
The selection of extracting method: adopt and add hot reflux, ultrasonic extraction respectively;
The selection of developping agent: respectively taking sherwood oil (60 DEG C～90 DEG C)-ethyl acetate (5: 1), sherwood oil (60 DEG C～90 DEG C)-ethyl acetate-formic acid (15: 5: 1) as developping agent.
(5) select respectively above different solvents, extracting method and developping agent to test, result is as follows:
Repetition test in the above conditions, finally determine that the specificity thin-layer identification method of Rhizoma Acori Calami is as follows:
Get described 18 taste asiabell preparation 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5: 1, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.As shown in Figure 3.The method operates through many people test of many times, favorable reproducibility, and specificity is strong, can be used as the detection method of 18 taste asiabell preparations.
Experimental example 4: the thin layer of frankincense is differentiated
(1) instrument
Mortar, electronic scales, tool plug conical flask, transfer pipet, ultrasound wave extraction apparatus, funnel, filter paper, evaporating dish, sample applicator, silica gel g thin-layer plate, chromatography cylinder, spray bottle, hair dryer.
(2) control medicinal material
Frankincense control medicinal material (lot number: 120970-200904), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
(3) reagent
Acetone, ethanol, normal hexane, cyclohexane, ethyl acetate, 5% vanillic aldehyde sulfuric acid solution.
(4) method of inspection:
Extract the selection of solvent: adopt respectively acetone and ethanol for extracting solvent;
The selection of extracting method: ultrasonic extraction and add hot reflux respectively;
The selection of developping agent: respectively taking normal hexane-ethyl acetate (9: 1), cyclohexane-ethyl acetate (9: 1) as developping agent.
(5) select respectively above different solvents, extracting method and developping agent to test, result is as follows:
Repetition test in the above conditions, finally determine that the specificity thin-layer identification method of the banksia rose is as follows:
Get described 18 taste asiabell preparation 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 9: 1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.As shown in Figure 4.The method operates through many people test of many times, favorable reproducibility, and specificity is strong, can be used as the detection method of 18 taste asiabell preparations.
Experimental example 5: aconitine limit inspection
(1) instrument
Mortar, electronic scales, tool plug conical flask, transfer pipet, ultrasound wave extraction apparatus, funnel, filter paper, evaporating dish, sample applicator, silica gel g thin-layer plate, chromatography cylinder, spray bottle, hair dryer.
(2) control medicinal material
Aconitine control medicinal material: (lot number: 110720-200410), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
(3) reagent
Ether, ammonia solution, methenyl choloride, sulfuric acid solution, absolute ethyl alcohol, toluene, benzene, cyclohexane, ethyl acetate, diethylamine, rare bismuth potassium iodide test solution, improvement bismuth potassium iodide test solution.
(4) extracting method
The selection of developping agent: respectively taking benzene-ethyl acetate-ethylenediamine (14: 4: 1), toluene-ethyl acetate-diethylamine (14: 4: 1), cyclohexane-ethyl acetate-ethylenediamine (14: 4: 1) as developping agent;
The selection of developer: respectively taking rare bismuth potassium iodide test solution and improvement bismuth potassium iodide test solution as colour developing.
(5) select respectively above different developping agents and developer to test, result is as follows:
Repetition test in the above conditions, finally determine that limit examine method is as follows:
Get described 18 taste asiabell preparation 5g, put in tool plug conical flask, 25mL adds diethyl ether, ammonia solution 3mL, close plug, shake up, place 24 hours, filter, the dregs of a decoction 50mL that adds diethyl ether, jolting 1 hour, filter, the dregs of a decoction are again with ether washing 2 times, each 15mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 10mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 10mL gradation washing container, washing lotion is incorporated in separating funnel, with 0.05mol/L sulfuric acid solution extraction 4 times, merge acid solution, add ammonia solution and regulate pH value to 9, extract 3 times with methenyl choloride again, merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 2mL to be made to dissolve, as need testing solution, it is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1mg, medicinal material solution in contrast, according to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, accurate need testing solution 5 μ L, the control medicinal material solution 5 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking volume ratio as the toluene-ethyl acetate-diethylamine of 14: 4: 1 is as developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.As shown in Figure 5.The method operates through many people test of many times, favorable reproducibility, and specificity is strong, can be used as the detection method of 18 taste asiabell preparations.
Following embodiment all can realize the effect of above-mentioned experimental example.
The discriminating of 1: ten eight taste Radix Codonopsis ball of embodiment
The 150g of ZANGDANGSHEN, tendril-leaved fritillary bulb 300g, cassia seed 80g, high mountain corydalis 10g, slag are tamed and dociled myrobalan 50g, hand ginseng 7.5g, terminaliae billericae,fructus 8.5g, Moschus 5g, frankincense 70g, Semen seu folium abelmoschi moschati 70g, styrax 50g, catechu 70g, BAXIAGA 70g, emblic 70g, the banksia rose 75g of cream 10g, Rhizoma Acori Calami 40g, wide muscle rattan 70g, stoning;
Above 18 tastes, tame and docile the another porphyrize powder of cream except Moschus, slag, and all the other are ground into fine powder altogether, sieve, and add muscone's fine powder, mix, and tame and docile cream add suitable quantity of water pill with slag, dry in the shade, and to obtain final product.
A. micro-discriminating
Get described 18 taste Radix Codonopsis balls, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.
B. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis ball 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 15: 5: 1 developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis ball 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5: 1, launch, and thin layer plate is put in expansion cylinder saturated 30 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis ball 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 9: 1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
E. the content inspection of aconitine
Get described 18 taste Radix Codonopsis ball 5g, porphyrize, put in tool plug conical flask, 25mL adds diethyl ether, ammonia solution 3mL, close plug, shake up, place 24 hours, filter, the dregs of a decoction 50mL that adds diethyl ether, jolting 1 hour, filter, the dregs of a decoction are again with ether washing 2 times, each 15mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 10mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 10mL gradation washing container, washing lotion is incorporated in separating funnel, with 4 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 9, extract 3 (20mL with methenyl choloride again, 15mL, 15mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 2mL to be made to dissolve, as need testing solution, it is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1mg, medicinal material solution in contrast, according to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, accurate need testing solution 5 μ L, the control medicinal material solution 5 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking volume ratio as the toluene-ethyl acetate-diethylamine of 14: 4: 1 is as developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 2: ten eight taste Radix Codonopsis capsules of embodiment
The 150g of ZANGDANGSHEN, tendril-leaved fritillary bulb 300g, cassia seed 80g, high mountain corydalis 10g, slag are tamed and dociled myrobalan 50g, hand ginseng 7.5g, terminaliae billericae,fructus 8.5g, Moschus 5g, frankincense 70g, Semen seu folium abelmoschi moschati 70g, styrax 50g, catechu 70g, BAXIAGA 70g, emblic 70g, the banksia rose 75g of cream 10g, Rhizoma Acori Calami 40g, wide muscle rattan 70g, stoning;
Above 18 tastes, except the another porphyrize powder of Moschus, all the other are ground into fine powder, sieve, and add Moschus fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis capsules clinically.
A. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis capsule 2g, porphyrize, adds methyl alcohol 20mL, and ultrasonic processing 45 minutes filters, and filtrate is concentrated into 3mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 7 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 20: 7: 1.8 developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
B. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis capsule 4.5g, porphyrize, the 20mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 45 minutes, filter, filtrate volatilizes, residue add diethyl ether 3mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.6g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 15 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=7: 1.5, and thin layer plate is put in expansion cylinder saturated 40 minutes, launches, and takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis capsule 0.5g, porphyrize, adds acetone 5mL, and ultrasonic processing 20 minutes filters, and filtrate is concentrated into 1mL, as need testing solution; Separately get frankincense control medicinal material 0.3g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 3 μ L, negative sample solution 5 μ L, control medicinal material solution 1 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 6: 0.8 is developping agent, and thin layer plate is put in expansion cylinder saturated 40 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the content inspection of aconitine
Get described 18 taste Radix Codonopsis capsule 2.5g, porphyrize, put in tool plug conical flask, 15mL adds diethyl ether, ammonia solution 2mL, close plug, shake up, place 12 hours, filter, the dregs of a decoction 40mL that adds diethyl ether, jolting constantly 0.5 hour, filter, the dregs of a decoction are again with ether washing 1 time, each 20mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 5mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 5mL gradation washing container, washing lotion is incorporated in separating funnel, with 3 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 8, extract 2 (20mL with methenyl choloride again, 15mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1mL to be made to dissolve, as need testing solution.It is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 0.5mg, medicinal material solution in contrast.Test according to thin-layered chromatography (annex VI B of " Chinese Pharmacopoeia " version in 2010), accurate need testing solution 4 μ L, the control medicinal material solution 4 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking toluene-ethyl acetate-diethylamine (12: 3: 0.6) as developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 3: ten eight taste Radix Codonopsis sheets of embodiment
The 180g of ZANGDANGSHEN, tendril-leaved fritillary bulb 200g, cassia seed 55g, high mountain corydalis 60g, slag are tamed and dociled myrobalan 175g, hand ginseng 60g, terminaliae billericae,fructus 110g, Moschus 0.5g, frankincense 90g, Semen seu folium abelmoschi moschati 95g, styrax 35g, catechu 90g, BAXIAGA 110g, emblic 90g, the banksia rose 115g of cream 40g, Rhizoma Acori Calami 170g, wide muscle rattan 90g, stoning;
Above 18 tastes, except the another porphyrize powder of Moschus, all the other are ground into fine powder, sieve, and add Moschus fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis sheets clinically.
A. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis sheet 1.5g, porphyrize, adds methyl alcohol 15mL, and ultrasonic processing 40 minutes filters, and filtrate is concentrated into 2.5mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 6 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 18: 6: 1.2 developping agent, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
B. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis sheet 4.5g, porphyrize, the 20mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 45 minutes, filter, filtrate volatilizes, residue add diethyl ether 3mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.6g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 15 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=7: 1.5, and thin layer plate is put in expansion cylinder saturated 40 minutes, launches, and takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis sheet 2.5g, porphyrize, adds acetone 20mL, and ultrasonic processing 45 minutes filters, and filtrate is concentrated into 3mL, as need testing solution; Separately get frankincense control medicinal material 0.6g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 3 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 12: 1.7 is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
The discriminating of 4: ten eight taste Radix Codonopsis particles of embodiment
The 150g of ZANGDANGSHEN, tendril-leaved fritillary bulb 300g, cassia seed 80g, high mountain corydalis 10g, slag are tamed and dociled myrobalan 50g, hand ginseng 7.5g, terminaliae billericae,fructus 8.5g, Moschus 5g, frankincense 70g, Semen seu folium abelmoschi moschati 70g, styrax 50g, catechu 70g, BAXIAGA 70g, emblic 70g, the banksia rose 75g of cream 10g, Rhizoma Acori Calami 40g, wide muscle rattan 70g, stoning;
Above 18 tastes, except the another porphyrize powder of Moschus, all the other are ground into fine powder, sieve, and add Moschus fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis particles clinically.
A. micro-discriminating
Get described 18 taste Radix Codonopsis particles, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.
B. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis particle 0.5g, porphyrize, adds methyl alcohol 5mL, and ultrasonic processing 20 minutes filters, and filtrate is concentrated into 1mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 3 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 12: 3: 0.8 developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis particle 4.5g, porphyrize, the 20mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 45 minutes, filter, filtrate volatilizes, residue add diethyl ether 3mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.6g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 15 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=7: 1.5, and thin layer plate is put in expansion cylinder saturated 40 minutes, launches, and takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis particle 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 9: 1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
The loose discriminating of 5: ten eight taste Radix Codonopsis of embodiment
The 150g of ZANGDANGSHEN, tendril-leaved fritillary bulb 300g, cassia seed 80g, high mountain corydalis 10g, slag are tamed and dociled myrobalan 50g, hand ginseng 7.5g, terminaliae billericae,fructus 8.5g, Moschus 5g, frankincense 70g, Semen seu folium abelmoschi moschati 70g, styrax 50g, catechu 70g, BAXIAGA 70g, emblic 70g, the banksia rose 75g of cream 10g, Rhizoma Acori Calami 40g, wide muscle rattan 70g, stoning;
Above 18 tastes, except the another porphyrize powder of Moschus, all the other are ground into fine powder, sieve, and add Moschus fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis clinically and fall apart.
A. the thin layer of the banksia rose is differentiated
Get the loose 1g of described 18 taste Radix Codonopsis, add methyl alcohol 10mL, ultrasonic processing 30 minutes, filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 15: 5: 1 developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
B. the thin layer of Rhizoma Acori Calami is differentiated
Get the loose 1.5g of described 18 taste Radix Codonopsis, the 5mL that adds diethyl ether, close plug, shakes up, and ultrasonic processing 20 minutes filters, and filtrate volatilizes, and the residue 2mL that adds diethyl ether makes to dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.2g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=3: 0.5, launch, and take out, dry, put under 254nm ultraviolet lamp and inspect.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of frankincense is differentiated
Get the loose 2.5g of described 18 taste Radix Codonopsis, add acetone 20mL, ultrasonic processing 45 minutes, filters, and filtrate is concentrated into 3mL, as need testing solution; Separately get frankincense control medicinal material 0.6g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 3 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 12: 1.7 is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the content inspection of aconitine
Get the loose 7.5g of described 18 taste Radix Codonopsis, put in tool plug conical flask, 40mL adds diethyl ether, ammonia solution 4mL, close plug, shake up, place 30 hours, filter, the dregs of a decoction 60mL that adds diethyl ether, jolting constantly 1.5 hours, filter, the dregs of a decoction are again with ether washing 3 times, each 10mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 20mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 20mL gradation washing container, washing lotion is incorporated in separating funnel, with 5 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 10, extract 4 (20mL with methenyl choloride again, 15mL, 10mL, 10mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1mL to be made to dissolve, as need testing solution.It is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1.5mg, medicinal material solution in contrast.Test according to thin-layered chromatography (annex VI B of " Chinese Pharmacopoeia " version in 2010), accurate need testing solution 6 μ L, the control medicinal material solution 6 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking toluene-ethyl acetate-diethylamine (17: 5: 1.8) as developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 6: ten eight taste Radix Codonopsis honeyed bolus of embodiment
The 220g of ZANGDANGSHEN, tendril-leaved fritillary bulb 100g, cassia seed 110g, high mountain corydalis 115g, slag are tamed and dociled myrobalan 105g, hand ginseng 110g, terminaliae billericae,fructus 8.65g, Moschus 9.5g, frankincense 70g110g, Semen seu folium abelmoschi moschati 70g55g, styrax 50g110g, catechu 70g40g, BAXIAGA 70g90g, emblic 70g110g, the banksia rose 75g55g of cream 75g, Rhizoma Acori Calami 100g, wide muscle rattan 110g, stoning;
Above 18 tastes, except the another porphyrize powder of Moschus, all the other are ground into fine powder, sieve, and add Moschus fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis honeyed bolus clinically.
A. micro-discriminating
Get described 18 taste Radix Codonopsis honeyed bolus, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.
B. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis honeyed bolus 0.5g, porphyrize, adds methyl alcohol 5mL, and ultrasonic processing 20 minutes filters, and filtrate is concentrated into 1mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 3 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 12: 3: 0.8 developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis honeyed bolus 2g, porphyrize, the 15mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 1mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.8g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 20 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=8: 1.8, launch, and thin layer plate is put in expansion cylinder saturated 20 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis honeyed bolus 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 9: 1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
E. the limit examine of aconitine
Get above-mentioned 18 taste Radix Codonopsis honeyed bolus 5g, porphyrize, put in tool plug conical flask, 25mL adds diethyl ether, ammonia solution 3mL, close plug, shake up, place 24 hours, filter, the dregs of a decoction 50mL that adds diethyl ether, jolting constantly 1 hour, filter, the dregs of a decoction are again with ether washing 2 times, each 15mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 10mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 10mL gradation washing container, washing lotion is incorporated in separating funnel, with 4 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 9, extract 3 (20mL with methenyl choloride again, 15mL, 15mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 2mL to be made to dissolve, as need testing solution.It is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1mg, medicinal material solution in contrast.Test according to thin-layered chromatography (annex VI B of " Chinese Pharmacopoeia " version in 2010), accurate need testing solution 5 μ L, the control medicinal material solution 5 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking toluene-ethyl acetate-diethylamine (14: 4: 1) as developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 7: ten eight taste Radix Codonopsis soft capsules of embodiment
The 150g of ZANGDANGSHEN, tendril-leaved fritillary bulb 300g, cassia seed 80g, high mountain corydalis 10g, slag are tamed and dociled myrobalan 50g, hand ginseng 7.5g, terminaliae billericae,fructus 8.5g, Moschus 5g, frankincense 70g, Semen seu folium abelmoschi moschati 70g, styrax 50g, catechu 70g, BAXIAGA 70g, emblic 70g, the banksia rose 75g of cream 10g, Rhizoma Acori Calami 40g, wide muscle rattan 70g, stoning;
Above 18 tastes, except the another porphyrize powder of Moschus, all the other are ground into fine powder, sieve, and add Moschus fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis soft capsules clinically.
A. micro-discriminating
Get described 18 taste Radix Codonopsis soft capsules, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.
B. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis soft capsule 1.5g, porphyrize, adds methyl alcohol 15mL, and ultrasonic processing 40 minutes filters, and filtrate is concentrated into 2.5mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 6 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 18: 6: 1.2 developping agent, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis soft capsule 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5: 1, launch, and thin layer plate is put in expansion cylinder saturated 30 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis soft capsule 3g, porphyrize, adds acetone 18mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.8g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 3 μ L, negative sample solution 3 μ L, control medicinal material solution 1 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 10: 1.5 is developping agent, and thin layer plate is put in expansion cylinder saturated 20 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
E. the limit examine of aconitine
Get above-mentioned 18 taste Radix Codonopsis soft capsule 2.5g, porphyrize, put in tool plug conical flask, 15mL adds diethyl ether, ammonia solution 2mL, close plug, shake up, place 12 hours, filter, the dregs of a decoction 40mL that adds diethyl ether, jolting constantly 0.5 hour, filter, the dregs of a decoction are again with ether washing 1 time, each 20mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 5mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 5mL gradation washing container, washing lotion is incorporated in separating funnel, with 3 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 8, extract 2 (20mL with methenyl choloride again, 15mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1mL to be made to dissolve, as need testing solution.It is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 0.5mg, medicinal material solution in contrast.Test according to thin-layered chromatography (annex VI B of " Chinese Pharmacopoeia " version in 2010), accurate need testing solution 4 μ L, the control medicinal material solution 4 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking toluene-ethyl acetate-diethylamine (12: 3: 0.6) as developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 8: ten eight taste Radix Codonopsis balls of embodiment
The 200g of ZANGDANGSHEN, that 100g of list, cassia seed 80g, Dong Siba 100g, slag are tamed and dociled myrobalan 150g, the hand of cream 50g, Rhizoma Acori Calami 150g, wide muscle rattan 100g, stoning and are joined cream 50g, BAXIAGA 100g, emblic 100g, the banksia rose 100g such as 100g, terminaliae billericae,fructus 100g, muscone 1.5g, frankincense 100g, Semen seu folium abelmoschi moschati 80g, bitter Kui Nabu 100g, Song Sheng;
Above 18 tastes, tame and docile the another porphyrize powder of cream except muscone, slag, and all the other are ground into fine powder altogether, sieve, and add muscone's fine powder, mix, and tame and docile cream add suitable quantity of water pill with slag, dry in the shade, and to obtain final product.
A. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis ball 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 15: 5: 1 developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
B. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis ball 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5: 1, launch, and thin layer plate is put in expansion cylinder saturated 30 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis ball 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 9: 1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the content inspection of aconitine
Get described 18 taste Radix Codonopsis ball 5g, porphyrize, put in tool plug conical flask, 25mL adds diethyl ether, ammonia solution 3mL, close plug, shake up, place 24 hours, filter, the dregs of a decoction 50mL that adds diethyl ether, jolting 1 hour, filter, the dregs of a decoction are again with ether washing 2 times, each 15mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 10mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 10mL gradation washing container, washing lotion is incorporated in separating funnel, with 4 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 9, extract 3 (20mL with methenyl choloride again, 15mL, 15mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 2mL to be made to dissolve, as need testing solution, it is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1mg, medicinal material solution in contrast, according to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, accurate need testing solution 5 μ L, the control medicinal material solution 5 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking volume ratio as the toluene-ethyl acetate-diethylamine of 14: 4: 1 is as developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 9: ten eight taste Radix Codonopsis capsules of embodiment
The 135g of ZANGDANGSHEN, that 300g of list, cassia seed 55g, Dong Siba 80g, slag are tamed and dociled myrobalan 105g, the hand of cream 10g, Rhizoma Acori Calami 95g, wide muscle rattan 60g, stoning and are joined cream 40g, BAXIAGA 60g, emblic 115g, the banksia rose 55g such as 10g, terminaliae billericae,fructus 65g, muscone 9g, frankincense 115g, Semen seu folium abelmoschi moschati 55g, bitter Kui Nabu 80g, Song Sheng;
Above 18 tastes, except the another porphyrize powder of muscone, all the other are ground into fine powder, sieve, and add muscone's fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis capsules clinically.
A. micro-discriminating
Get described 18 taste Radix Codonopsis capsules, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.
B. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis capsule 0.5g, porphyrize, adds methyl alcohol 5mL, and ultrasonic processing 20 minutes filters, and filtrate is concentrated into 1mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 3 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 12: 3: 0.8 developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis capsule 1.5g, porphyrize, the 5mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 20 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.2g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=3: 0.5, launch, and take out, dry, put under 254nm ultraviolet lamp and inspect.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis capsule 0.5g, porphyrize, adds acetone 5mL, and ultrasonic processing 20 minutes filters, and filtrate is concentrated into 1mL, as need testing solution; Separately get frankincense control medicinal material 0.3g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 3 μ L, negative sample solution 5 μ L, control medicinal material solution 1 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 6: 0.8 is developping agent, and thin layer plate is put in expansion cylinder saturated 40 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
The discriminating of 10: ten eight taste Radix Codonopsis sheets of embodiment
The 200g of ZANGDANGSHEN, that 100g of list, cassia seed 80g, Dong Siba 100g, slag are tamed and dociled myrobalan 150g, the hand of cream 50g, Rhizoma Acori Calami 150g, wide muscle rattan 100g, stoning and are joined cream 50g, BAXIAGA 100g, emblic 100g, the banksia rose 100g such as 100g, terminaliae billericae,fructus 100g, muscone 1.5g, frankincense 100g, Semen seu folium abelmoschi moschati 80g, bitter Kui Nabu 100g, Song Sheng;
Above 18 tastes, except the another porphyrize powder of muscone, all the other are ground into fine powder, sieve, and add muscone's fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis sheets clinically.
A. micro-discriminating
Get described 18 taste Radix Codonopsis sheets, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.
B. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis sheet 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 15: 5: 1 developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis sheet 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5: 1, launch, and thin layer plate is put in expansion cylinder saturated 30 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis sheet 2.5g, porphyrize, adds acetone 20mL, and ultrasonic processing 45 minutes filters, and filtrate is concentrated into 3mL, as need testing solution; Separately get frankincense control medicinal material 0.6g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 3 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 12: 1.7 is developping agent, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
E. the content inspection of aconitine
Get described 18 taste Radix Codonopsis sheet 2.5g, porphyrize, put in tool plug conical flask, 15mL adds diethyl ether, ammonia solution 2mL, close plug, shake up, place 12 hours, filter, the dregs of a decoction 40mL that adds diethyl ether, jolting constantly 0.5 hour, filter, the dregs of a decoction are again with ether washing 1 time, each 20mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 5mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 5mL gradation washing container, washing lotion is incorporated in separating funnel, with 3 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 8, extract 2 (20mL with methenyl choloride again, 15mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1mL to be made to dissolve, as need testing solution.It is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 0.5mg, medicinal material solution in contrast.Test according to thin-layered chromatography (annex VI B of " Chinese Pharmacopoeia " version in 2010), accurate need testing solution 4 μ L, the control medicinal material solution 4 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking toluene-ethyl acetate-diethylamine (12: 3: 0.6) as developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 11: ten eight taste Radix Codonopsis particles of embodiment
The 235g of ZANGDANGSHEN, that 200g of list, cassia seed 115g, Dong Siba 10g, slag are tamed and dociled myrobalan 30g, the hand of cream 75g, Rhizoma Acori Calami 30g, wide muscle rattan 115g, stoning and are joined cream 90g, BAXIAGA 115g, emblic 55g, the banksia rose 115g such as 60g, terminaliae billericae,fructus 10g, muscone 4.5g, frankincense 60g, Semen seu folium abelmoschi moschati 95g, bitter Kui Nabu 35g, Song Sheng;
Above 18 tastes, except the another porphyrize powder of muscone, all the other are ground into fine powder, sieve, and add muscone's fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis particles clinically.
A. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis particle 2g, porphyrize, adds methyl alcohol 20mL, and ultrasonic processing 45 minutes filters, and filtrate is concentrated into 3mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 7 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 20: 7: 1.8 developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
B. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis particle 2g, porphyrize, the 15mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 1mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.8g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 20 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=8: 1.8, launch, and thin layer plate is put in expansion cylinder saturated 20 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis particle 3g, porphyrize, adds acetone 18mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.8g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 3 μ L, negative sample solution 3 μ L, control medicinal material solution 1 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 10: 1.5 is developping agent, and thin layer plate is put in expansion cylinder saturated 20 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the content inspection of aconitine
Get described 18 taste Radix Codonopsis particle 7.5g, porphyrize, put in tool plug conical flask, 40mL adds diethyl ether, ammonia solution 4mL, close plug, shake up, place 30 hours, filter, the dregs of a decoction 60mL that adds diethyl ether, jolting constantly 1.5 hours, filter, the dregs of a decoction are again with ether washing 3 times, each 10mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 20mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 20mL gradation washing container, washing lotion is incorporated in separating funnel, with 5 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 10, extract 4 (20mL with methenyl choloride again, 15mL, 10mL, 10mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1mL to be made to dissolve, as need testing solution.It is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1.5mg, medicinal material solution in contrast.Test according to thin-layered chromatography (annex VI B of " Chinese Pharmacopoeia " version in 2010), accurate need testing solution 6 μ L, the control medicinal material solution 6 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking toluene-ethyl acetate-diethylamine (17: 5: 1.8) as developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The loose discriminating of 12: ten eight taste Radix Codonopsis of embodiment
The 200g of ZANGDANGSHEN, that 100g of list, cassia seed 80g, Dong Siba 100g, slag are tamed and dociled myrobalan 150g, the hand of cream 50g, Rhizoma Acori Calami 150g, wide muscle rattan 100g, stoning and are joined cream 50g, BAXIAGA 100g, emblic 100g, the banksia rose 100g such as 100g, terminaliae billericae,fructus 100g, muscone 1.5g, frankincense 100g, Semen seu folium abelmoschi moschati 80g, bitter Kui Nabu 100g, Song Sheng;
Above 18 tastes, except the another porphyrize powder of muscone, all the other are ground into fine powder, sieve, and add muscone's fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis clinically and fall apart.
A. the thin layer of the banksia rose is differentiated
Get the loose 1.5g of described 18 taste Radix Codonopsis, add methyl alcohol 15mL, ultrasonic processing 40 minutes, filters, and filtrate is concentrated into 2.5mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 6 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 18: 6: 1.2 developping agent, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
B. the thin layer of Rhizoma Acori Calami is differentiated
Get the loose 2g of described 18 taste Radix Codonopsis, the 15mL that adds diethyl ether, close plug, shakes up, and ultrasonic processing 30 minutes filters, and filtrate volatilizes, and the residue 1mL that adds diethyl ether makes to dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.8g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 20 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=8: 1.8, launch, and thin layer plate is put in expansion cylinder saturated 20 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of frankincense is differentiated
Get the loose 0.5g of described 18 taste Radix Codonopsis, add acetone 5mL, ultrasonic processing 20 minutes, filters, and filtrate is concentrated into 1mL, as need testing solution; Separately get frankincense control medicinal material 0.3g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 3 μ L, negative sample solution 5 μ L, control medicinal material solution 1 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 6: 0.8 is developping agent, and thin layer plate is put in expansion cylinder saturated 40 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
The discriminating of 13: ten eight taste Radix Codonopsis honeyed bolus of embodiment
The 200g of ZANGDANGSHEN, that 100g of list, cassia seed 80g, Dong Siba 100g, slag are tamed and dociled myrobalan 150g, the hand of cream 50g, Rhizoma Acori Calami 150g, wide muscle rattan 100g, stoning and are joined cream 50g, BAXIAGA 100g, emblic 100g, the banksia rose 100g such as 100g, terminaliae billericae,fructus 100g, muscone 1.5g, frankincense 100g, Semen seu folium abelmoschi moschati 80g, bitter Kui Nabu 100g, Song Sheng;
Above 18 tastes, except the another porphyrize powder of muscone, all the other are ground into fine powder, sieve, and add muscone's fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis honeyed bolus clinically.
A. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis honeyed bolus 2g, porphyrize, adds methyl alcohol 20mL, and ultrasonic processing 45 minutes filters, and filtrate is concentrated into 3mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 7 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 20: 7: 1.8 developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
B. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis honeyed bolus 1.5g, porphyrize, the 5mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 20 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.2g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=3: 0.5, launch, and take out, dry, put under 254nm ultraviolet lamp and inspect.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis honeyed bolus 3g, porphyrize, adds acetone 18mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.8g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 3 μ L, negative sample solution 3 μ L, control medicinal material solution 1 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 10: 1.5 is developping agent, and thin layer plate is put in expansion cylinder saturated 20 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the limit examine of aconitine
Get above-mentioned 18 taste Radix Codonopsis honeyed bolus 2.5g, porphyrize, put in tool plug conical flask, 15mL adds diethyl ether, ammonia solution 2mL, close plug, shake up, place 12 hours, filter, the dregs of a decoction 40mL that adds diethyl ether, jolting constantly 0.5 hour, filter, the dregs of a decoction are again with ether washing 1 time, each 20mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 5mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 5mL gradation washing container, washing lotion is incorporated in separating funnel, with 3 (20mL of 0.05mol/L sulfuric acid solution extraction, 10mL, 10mL), merge acid solution, add ammonia solution and regulate pH value to 8, extract 2 (20mL with methenyl choloride again, 15mL), merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1mL to be made to dissolve, as need testing solution.It is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 0.5mg, medicinal material solution in contrast.Test according to thin-layered chromatography (annex VI B of " Chinese Pharmacopoeia " version in 2010), accurate need testing solution 4 μ L, the control medicinal material solution 4 μ L of drawing, put respectively on same silica gel g thin-layer plate, taking toluene-ethyl acetate-diethylamine (12: 3: 0.6) as developping agent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
The discriminating of 14: ten eight taste Radix Codonopsis soft capsules of embodiment
The 200g of ZANGDANGSHEN, that 100g of list, cassia seed 80g, Dong Siba 100g, slag are tamed and dociled myrobalan 150g, the hand of cream 50g, Rhizoma Acori Calami 150g, wide muscle rattan 100g, stoning and are joined cream 50g, BAXIAGA 100g, emblic 100g, the banksia rose 100g such as 100g, terminaliae billericae,fructus 100g, muscone 1.5g, frankincense 100g, Semen seu folium abelmoschi moschati 80g, bitter Kui Nabu 100g, Song Sheng;
Above 18 tastes, except the another porphyrize powder of muscone, all the other are ground into fine powder, sieve, and add muscone's fine powder, mix, and by pharmacy conventional method, add conventional auxiliary material, make acceptable 18 taste Radix Codonopsis soft capsules clinically.
A. micro-discriminating
Get described 18 taste Radix Codonopsis soft capsules, porphyrize, adds chloral hydrate and thoroughly changes 1-3 time, and micro-Microscopic observation is put in film-making, differentiates the morphological feature of ingredients:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of bitter Kui Nabu: resin crystallization is unsetting, and rufous is translucent, and corner angle are obvious;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells.
B. the thin layer of the banksia rose is differentiated
Get described 18 taste Radix Codonopsis soft capsule 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is to be at 15: 5: 1 developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
C. the thin layer of Rhizoma Acori Calami is differentiated
Get described 18 taste Radix Codonopsis soft capsule 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5: 1, launch, and thin layer plate is put in expansion cylinder saturated 30 minutes, takes out, and dries, and puts under 254nm ultraviolet lamp and inspects.In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.
D. the thin layer of frankincense is differentiated
Get described 18 taste Radix Codonopsis soft capsule 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution.According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that the cyclohexane-ethyl acetate of 9: 1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing.In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram.

Claims (7)

1. the detection method of a taste asiabell preparation, said preparation bulk drug consists of: the 120-240 of ZANGDANGSHEN weight portion, that 80-320 weight portion of tendril-leaved fritillary bulb/list, cassia seed 50-120 weight portion, high mountain corydalis/Dong Siba 5-120 weight portion, slag is tamed and dociled cream 5-80 weight portion, Rhizoma Acori Calami 20-180 weight portion, wide muscle rattan 50-120 weight portion, the myrobalan 25-180 weight portion of stoning, hand ginseng 1-120 weight portion, terminaliae billericae,fructus 1-120 weight portion, Moschus/muscone 0.1-10 weight portion, frankincense 50-120 weight portion, Semen seu folium abelmoschi moschati 50-100 weight portion, styrax 30-120 weight portion, the cream 30-100 weight portions such as catechu/Song Sheng, BAXIAGA 50-120 weight portion, emblic 50-120 weight portion, banksia rose 50-120 weight portion,
The method comprises following discriminating and inspection method:
When existing list at that time in preparation, by microscope differentiate preparation Chinese crude drug ZANGDANGSHEN, list that, the morphological feature of cassia seed, Rhizoma Acori Calami, wide muscle rattan, myrobalan, hand ginseng, terminaliae billericae,fructus, frankincense, BAXIAGA;
In the time there is tendril-leaved fritillary bulb in preparation, differentiate the morphological feature of preparation Chinese crude drug ZANGDANGSHEN, cassia seed, Rhizoma Acori Calami, wide muscle rattan, myrobalan, hand ginseng, terminaliae billericae,fructus, frankincense, BAXIAGA by microscope;
By thin-layer chromatography, the banksia rose in preparation, Rhizoma Acori Calami, frankincense are carried out to qualitative discriminating, and check preparation mesaconitine content;
Wherein, described microscope is differentiated and is comprised:
Get described 18 taste asiabell preparations and put micro-Microscopic observation, differentiate the morphological feature of following ingredients, wherein:
The Main Morphology feature of ZANGDANGSHEN: have joint connecting lactiferous duct, diameter 12～15 μ m, are full of oily drop and fine grained in laticifer and in peripheral cell; Synanthrin is fan-shaped, the existing radial texture in surface;
That Main Morphology feature of list: amylum body is numerous, simple grain is that class is spherical, polygon or helmet hat, diameter 4～11 μ m, omphalion is obvious, is point-like, starlike or crack shape, 2～5 compositions of composite grain;
The Main Morphology feature of cassia seed: how in blocks seed coat palisade cells is, colourless or faint yellow, surface is seen and is class polygon, the micro-shrinkage of wall;
The Main Morphology feature of Rhizoma Acori Calami: the normal bunchy of fiber, minority is dispersed in, the single spindle shape that is, end is point gradually;
The Main Morphology feature of wide muscle rattan: pericyclic fiber is slightly thick, normal containing calcium oxalate prismatic crystal in parenchyma cell around, form crystal fiber;
Myrobalan's Main Morphology feature: lithocyte in groups, is similar round, long avette, rectangle or strip, and hole ditch is fine and closely woven and clear, and mesocarp parenchyma cell similar round, includes calcium oxalate cluster crystal;
The Main Morphology feature of hand ginseng: needle-like calcium oxalate crystal is easily shown in, in parenchyma cell, bunchy is dispersed in;
The Main Morphology feature of terminaliae billericae,fructus: nonglandular hair 1-2 cell, have containing yellow or yellowish-brown thing;
The Main Morphology feature of frankincense: irregular agglomerate is colourless or faint yellow, surface and diffuse out numerous fine particles around, be long placed in and dissolve;
The Main Morphology feature of BAXIAGA: leaf epicuticle cell anticline is straight, has nonglandular hair trace, pore infinitive, 4～5 of accessory cells;
The qualitative discriminating of the banksia rose comprises:
1a) prepare the negative sample solution that the banksia rose is determined need testing solution, banksia rose control medicinal material solution, do not contained the banksia rose;
2a), according to 2010 editions one annex VI B of thin-layered chromatography " Chinese Pharmacopoeia " test, draw respectively step 1a) need testing solution, control medicinal material solution, the negative sample solution that obtain, and point sample is on same silica gel g thin-layer plate;
3a) taking cyclohexane-methylene chloride-ethyl acetate as developping agent, by step 2a) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, spray is with vanillic aldehyde sulfuric acid solution, wind is clear to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
The qualitative discriminating of Rhizoma Acori Calami comprises:
1b) prepare the need testing solution, Rhizoma Acori Calami control medicinal material solution of Rhizoma Acori Calami, not containing the negative sample solution of Rhizoma Acori Calami;
2b), according to 2010 editions one annex VI B of thin-layered chromatography " Chinese Pharmacopoeia " test, draw respectively step 1b) need testing solution, control medicinal material solution, the negative sample solution that obtain, and point sample is on same silica gel g thin-layer plate;
3b) taking petroleum ether-ethyl acetate as developping agent, by step 2b) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, put under ultraviolet lamp and inspect; In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
The qualitative discriminating of frankincense comprises:
1c) prepare the need testing solution, frankincense control medicinal material solution of frankincense, not containing the negative sample solution of frankincense;
2c), according to 2010 editions one annex VI B of thin-layered chromatography " Chinese Pharmacopoeia " test, draw respectively step 1c) need testing solution, control medicinal material solution, the negative sample solution that obtain, and point sample is on same silica gel g thin-layer plate;
3c) taking cyclohexane-ethyl acetate as developping agent, by step 2c) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, wind is clear to spot colour developing; In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
Content of Aconitine inspection comprises:
1d) prepare need testing solution, the aconitine control medicinal material solution of aconitine;
2d), according to annex VI B test of thin-layered chromatography " Chinese Pharmacopoeia " version in 2010, draw respectively step 1d) need testing solution, the aconitine control medicinal material solution that obtain, and point sample is on same silica gel g thin-layer plate;
3d) taking toluene-ethyl acetate-diethylamine as developping agent, by step 2d) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, spray is with rare bismuth potassium iodide test solution; In thin-layer chromatography, test sample chromatogram with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
2. detection method as claimed in claim 1, the preparation method of the need testing solution of the wherein said banksia rose, Rhizoma Acori Calami, frankincense and aconitine, control medicinal material solution, negative sample solution comprises:
(1) need testing solution of the banksia rose, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, porphyrize, adds methyl alcohol, and ultrasonic processing filters, and filtrate is concentrated, as the need testing solution of the banksia rose; Separately get dehydro-α-curcumene control medicinal material, be made in the same way of banksia rose control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution;
(2) need testing solution of Rhizoma Acori Calami, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, porphyrize, adds diethyl ether, and ultrasonic processing filters, and filtrate volatilizes, and residue adds diethyl ether and makes to dissolve, as the need testing solution of Rhizoma Acori Calami; Separately get Rhizoma Acori Calami control medicinal material, be made in the same way of Rhizoma Acori Calami control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution;
(3) need testing solution of frankincense, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, porphyrize, adds acetone, and ultrasonic processing filters, and filtrate is concentrated into, as the need testing solution of frankincense; Separately get frankincense control medicinal material, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution;
(4) need testing solution of aconitine, control medicinal material solution, negative sample solution
Get described 18 taste asiabell preparations, put in tool plug conical flask, add diethyl ether, ammonia solution, close plug, shake up, place, filter, the dregs of a decoction add diethyl ether, jolting, filter, the dregs of a decoction wash with ether again, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride to be made to dissolve, be transferred in separating funnel, with methenyl choloride gradation washing container, washing lotion is incorporated in separating funnel, extract with 0.05mol/L sulfuric acid solution, merge acid solution, add ammonia solution and regulate pH value extremely, extract with methenyl choloride again, merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol to be made to dissolve, as the need testing solution of aconitine, separately get aconitine control medicinal material, add absolute ethyl alcohol and make control medicinal material solution.
3. the detection method as described in claim 1 to 2 any one, comprises the steps:
A) the qualitative discriminating of the banksia rose
Get described 18 taste asiabell preparation 0.5～2 weight portions, porphyrize, adds methyl alcohol 5～20 parts by volume, and ultrasonic processing 20～45 minutes filters, and filtrate is concentrated into 1～3 parts by volume, as the need testing solution of the banksia rose; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every parts by volume containing 0.0005 weight portion; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution; According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw each 0.003～0.007 parts by volume of above-mentioned three kinds of solution, point sample is on same silica gel g thin-layer plate respectively, and with cyclohexane-methylene chloride-ethyl acetate, volume ratio is that 10～20:2～8:0.5～2 are developping agent, thin layer plate is put in expansion cylinder saturated 0～40 minute, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
B) the qualitative discriminating of Rhizoma Acori Calami
Get described 18 taste asiabell preparation 1～5 weight portions, porphyrize, 5～20 parts by volume that add diethyl ether, close plug, shakes up, ultrasonic processing 20～45 minutes, filter, filtrate volatilizes, residue add diethyl ether 1～3 parts by volume make dissolve, as the need testing solution of Rhizoma Acori Calami; Separately get Rhizoma Acori Calami control medicinal material 0.1～0.8 weight portion, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution; According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw each 0.005～0.02 parts by volume of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as 60 DEG C～90 DEG C petroleum ether-ethyl acetates are as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=2～8:0.5～2, thin layer plate is put in expansion cylinder saturated 0～40 minute, launches, and takes out, dry, put under 254nm ultraviolet lamp and inspect; In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
C) the qualitative discriminating of frankincense
Get described 18 taste asiabell preparation 0.5～3 weight portions, porphyrize, adds acetone 5～20 parts by volume, and ultrasonic processing 20～45 minutes filters, and filtrate is concentrated into 1～3 parts by volume, as the need testing solution of frankincense; Separately get frankincense control medicinal material 0.1～0.8 weight portion, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution; According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 0.003～0.007 parts by volume, negative sample solution 0.003～0.007 parts by volume, control medicinal material solution 0.001～0.003 parts by volume, put respectively on same silica gel g thin-layer plate, taking volume ratio as 5～15: cyclohexane-ethyl acetate of 0.5～2 is developping agent, thin layer plate is put in expansion cylinder saturated 0～40 minute, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
D) the content inspection of aconitine
Get described 18 taste asiabell preparation 2～8 weight portions, put in tool plug conical flask, 15～40 parts by volume add diethyl ether, ammonia solution 1～5 parts by volume, close plug, shake up, place 18～30 hours, filter, the dregs of a decoction 30～70 parts by volume that add diethyl ether, jolting 0.5～2 hour, filter, the dregs of a decoction are again with ether washing 1～3 time, each 5～25 parts by volume, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 5～20 parts by volume to be made to dissolve, be transferred in separating funnel, with methenyl choloride 5～20 parts by volume gradation washing containers, washing lotion is incorporated in separating funnel, with 0.05mol/L sulfuric acid solution extraction 2～6 times, merge acid solution, add ammonia solution and regulate pH value to 7～11, extract 2～5 times with methenyl choloride again, merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 1～3 parts by volume to be made to dissolve, as the need testing solution of aconitine, it is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every parts by volume containing 0.0005～0.002 weight portion, medicinal material solution in contrast, according to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, accurate need testing solution 0.003～0.007 parts by volume, control medicinal material solution 0.003～0.007 parts by volume drawn, put respectively on same silica gel g thin-layer plate, toluene-ethyl acetate-diethylamine taking volume ratio as 10～20:2～6:0.5～2 is developping agent, thin layer plate is put in expansion cylinder saturated 0～40 minute, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
4. detection method as claimed in claim 3, comprises the following steps:
I) the qualitative discriminating of the banksia rose:
Get described 18 taste asiabell preparation 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as the need testing solution of the banksia rose; Separately get dehydro-α-curcumene control medicinal material, add methyl alcohol and make the control medicinal material solution of every 1mL containing 0.5mg; In prescription ratio and preparation technology, configuration does not contain the negative sample of the banksia rose, and makes the not negative sample solution containing the banksia rose by the preparation method of described need testing solution; According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-methylene chloride-ethyl acetate, volume ratio is that 15:5:1 is developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of banksia rose control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
Ii) the qualitative discriminating of Rhizoma Acori Calami:
Get described 18 taste asiabell preparation 3g, porphyrize, the 10mL that adds diethyl ether, close plug, shakes up, ultrasonic processing 30 minutes, filter, filtrate volatilizes, residue add diethyl ether 2mL make dissolve, as need testing solution; Separately get Rhizoma Acori Calami control medicinal material 0.4g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of Rhizoma Acori Calami, and makes the not negative sample solution containing Rhizoma Acori Calami by the preparation method of described need testing solution; According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw the each 10 μ L of above-mentioned three kinds of solution, put respectively in same silica G F 254on thin layer plate, taking boiling point as the petroleum ether-ethyl acetate of 60 DEG C～90 DEG C is as developping agent, the volume ratio of developping agent is sherwood oil: ethyl acetate=5:1, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, and dries, and puts under 254nm ultraviolet lamp and inspects; In thin-layer chromatography, with the corresponding position of Rhizoma Acori Calami control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
Iii) the qualitative discriminating of frankincense
Get described 18 taste asiabell preparation 1g, porphyrize, adds acetone 10mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 2mL, as need testing solution; Separately get frankincense control medicinal material 0.5g, be made in the same way of control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of frankincense, and makes the not negative sample solution containing frankincense by the preparation method of described need testing solution; According to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, draw need testing solution 5 μ L, negative sample solution 5 μ L, control medicinal material solution 2 μ L, put respectively on same silica gel g thin-layer plate, volume ratio is that cyclohexane-ethyl acetate of 9:1 is developping agent, and thin layer plate is put in expansion cylinder saturated 30 minutes, launches, take out, dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to spot colour developing; In thin-layer chromatography, with the corresponding position of frankincense control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
Iv) the content inspection of aconitine
Get described 18 taste asiabell preparation 5g, put in tool plug conical flask, 25mL adds diethyl ether, ammonia solution 3mL, close plug, shake up, place 24 hours, filter, the dregs of a decoction 50mL that adds diethyl ether, jolting 1 hour, filter, the dregs of a decoction are again with ether washing 2 times, each 15mL, filter, merge above-mentioned filtrate and washing lotion, evaporate to dryness, residue adds methenyl choloride 10mL to be made to dissolve, be transferred in separating funnel, with methenyl choloride 10mL gradation washing container, washing lotion is incorporated in separating funnel, with 0.05mol/L sulfuric acid solution extraction 4 times, merge acid solution, add ammonia solution and regulate pH value to 9, extract 3 times with methenyl choloride again, merge methenyl choloride liquid, low temperature evaporate to dryness, residue adds absolute ethyl alcohol 2mL to be made to dissolve, as need testing solution, it is appropriate that precision takes aconitine control medicinal material, adds absolute ethyl alcohol and make the solution of every 1mL containing 1mg, medicinal material solution in contrast, according to thin-layered chromatography test described in annex VI B of " Chinese Pharmacopoeia " version in 2010, accurate need testing solution 5 μ L, the control medicinal material solution 5 μ L of drawing, put respectively on same silica gel g thin-layer plate, toluene-ethyl acetate-diethylamine taking volume ratio as 14:4:1 is developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on the spot that occurs should be less than the spot of control medicinal material or not occur spot.
5. the detection method as described in claim 1～2 any one, it is characterized in that, described preparation raw material medicine consists of: ZANGDANGSHEN's 150 weight portions, tendril-leaved fritillary bulb 300 weight portions, cassia seed 80 weight portions, high mountain corydalis 10 weight portions, slag is tamed and dociled cream 10 weight portions, Rhizoma Acori Calami 40 weight portions, wide muscle rattan 70 weight portions, myrobalan's 50 weight portions of stoning, hand is joined 7.5 weight portions, terminaliae billericae,fructus 8.5 weight portions, Moschus 5 weight portions, frankincense 70 weight portions, Semen seu folium abelmoschi moschati 70 weight portions, styrax 50 weight portions, catechu 70 weight portions, BAXIAGA 70 weight portions, emblic 70 weight portions, the banksia rose 75 weight portions.
6. the detection method as described in claim 1～2 any one, is characterized in that, the formulation of described 18 taste asiabell preparations is tablet, capsule, granule, pill or powder.
7. the detection method as described in claim 1～2 any one, is characterized in that, gets described 18 taste asiabell preparations, is ground into fine powder, sieves, and mixes, and adds suitable quantity of water pill, dries in the shade and get final product; Or get described 18 taste asiabell preparations, and be ground into fine powder, sieve, mix, mix, by pharmacy conventional method, add conventional auxiliary material, make the oral formulations of accepting clinically.
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