CN102590430B - Method for detecting liuwei caragana preparation - Google Patents
Method for detecting liuwei caragana preparation Download PDFInfo
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Abstract
The invention relates to a method for detecting a liuwei caragana preparation, which comprises the following identification method of qualitatively identifying phyllanthus emblica and/or lagotisglauca in the preparation through thin layer chromatography. The detecting method has the characteristics of good sensitivity and reproducibility and strong specificity. The liuwei caragana preparation can be effectively detected through the detecting method.
Description
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
Six-element caragana soup falls apart for Tibetan medicine, record in < < the Sanitation Ministry medicine standard > > Tibetan medicine fascicle, standard number is WS3-BC-0292-95, shagspine peashrub bark stem and leaf, Tibet inula root, tsaoko, cardamom, betel nut, galangal Six-element medicine, consists of.Be mainly used in concocting blood, dragon, cough, is short of breath, kidney Low Back Pain pain, seminal emission, private parts fistula that internal lesion caused by overexertion causes, and " ridge bar " is sick, ascites.
The Six-element caragana soup random notes of using are at present loaded in first of < < Drug Standard of Ministry of Public Health of the Peoples Republic of China > > nineteen ninety-five version Tibetan medicine:
Phonetic name: Liuwei Jinjier Tangsan
Book page number: C1-295 standard number: WS3-BC-0292-95
[prescription] shagspine peashrub bark stem and leaf 200g, Tibet inula root 200g, tsaoko 100g, cardamom 100g, betel nut 100g, galangal 100g.
[method for making] above Six-element, is ground into meal, sieves, and mixes, and obtains.
[proterties] this product is light brown meal; The micro-perfume (or spice) of gas, bitter, micro-peppery.
[inspection] should meet every regulation relevant under powder item.
[function with cure mainly] kidney tonifying, eliminating dampness.Be used for concocting blood, dragon, cough, is short of breath, kidney Low Back Pain pain, seminal emission, private parts fistula that internal lesion caused by overexertion causes, and " ridge bar " is sick, ascites.
[usage and consumption] 2g, 2 times on the one.Use milk tea decoction.
[specification] every packed 20g.
[storage] is airtight, puts shady and cool dry place.
The requirement that the present invention improves according to Tibetan medicine quality standard, adjusts this prescription Chinese crude drug and dosage, is specially: the cream 100g such as ZANGJINJIER 150g, BAXIAGA 100g, emblic 130g, Herba Corydalis 100g, Song Sheng, flood connect 100g.
ZANGJINJIER: record < < the Sanitation Ministry medicine standard > > (first of Tibetan medicine), this product is the woody part heartwood of legume shagspine peashrub bark stem and leaf Caraganajubata (pall.) Poir. and Changdu caragana Caraganachangduensis fiauf.Cut and get maroon woody part, cut off, dry in the shade.
BAXIAGA: record the local quality of medicinal material standard > > in < < Tibet Autonomous Region, standard No. is XZ-BC-0001-2003, for the dry aerial parts of bloodroot C. racemosa Corydalis racemosa (Thunb.) pers, dry or cut off dry standby.
Emblic: record one of < < Chinese Pharmacopoeia > > version in 2010, the 167th page, this strain Tibetan conventional crude drugs is the dry mature fruit of euphorbia plant emblic Phyllanthus emblica L..Winter to time spring gathers during fruit maturation, removes impurity, dry.
Herba Corydalis: record in < < the Sanitation Ministry medicine standard > > (first of Tibetan medicine), standard number: WS3-BC-0114-95, this product is the dry herb of bloodroot Herba Corydalis Corydalis hendersonii Hemsl. (C.nepaiesis kitamura) and the yellow violet C.mucionifera of flat handle Maxim., grubbed out summer, clean, dry in the shade.
Hong Lian: record one of < < Chinese Pharmacopoeia > > version in 2010, the 249th page, this strain Tibetan conventional crude drugs.Dry herb for the short cylinder of goatweed Lagotis glauca Lagotis brevituba Maxim.Summer, autumn gathered when two seasons, the flowers are in blossom, removed impurity, cleaned, and dried in the shade.
The cream such as Song Sheng: this product is the desiccated wood of the Fructus Rhamni parvifoliae Rhamnus parvifolia Bunge of Rhamnaceae plant Rhamnella gilgitica Rhamnella gilgitica Mansf.et Melch..All can gather the whole year, and except debarking, the section of being sawn into, dries after riving.The material sheet of getting it filled, adds 2 times, water, with Wenshui, simmers bubble 3～4 days, boils 4 hours, filters, and residue adds 1.5 times, water again, boils, filters secondary, and merging filtrate, is condensed into cream with slow fire.
Tsaoko: record one of < < Chinese Pharmacopoeia > > version in 2010, the 222nd page, this product is the dry mature fruit of zingiberaceous plant tsaoko Amomum tsao-ko Crevost et Lemaire.Gather during fruit maturation autumn, removes impurity, dries or low temperature drying.
Cardamom: record one of < < Chinese Pharmacopoeia > > version in 2010, the 156th page, this product is the dry mature fruit of zingiberaceous plant Amomum cardamomum Amomum Kravanh Pierre exGagnep. or amomum compactum Soland ex Maton Amomum compactum Soland ex Maton.By place of production difference, be divided into " former cardamom " and " the white bandit of Indonesia ".
Betel nut: record one of < < Chinese Pharmacopoeia > > version in 2010, the 342nd page, this product is the dry mature seed of babassu betel nut Rreca catechu L..The ripening fruits of gathering at the beginning of spring end to autumn, with after poach, dry, remove pericarp, take out seed, dry.
Galangal: record one of < < Chinese Pharmacopoeia > > version in 2010, the 270th page, this product is the dry rhizome of zingiberaceous plant galangal Alpinia officinarum Hance.At the beginning of autumn late summer, excavate, remove fibrous root and residual scale, clean, cut off, dry.
The detection method that not yet has at present Six-element caragana preparation.
Summary of the invention
The object of the present invention is to provide a kind of detection method of Six-element caragana preparation, described method favorable reproducibility, specificity are strong, can effectively detect the quality of Six-element caragana preparation, thereby make the steady quality, safe, controlled of Six-element caragana preparation.
For achieving the above object, technical scheme of the present invention is:
A detection method for Six-element caragana preparation, the bulk drug of described preparation consists of: the cream 80-120 weight portions such as ZANGJINJIER/shagspine peashrub bark stem and leaf 120-180 weight portion, BAXIAGA 80-120 weight portion, emblic 100-150 weight portion, Herba Corydalis 80-120 weight portion, Song Sheng, flood connect 80-120 weight portion;
Described detection method comprises:
By thin-layer chromatography, the emblic in preparation and/or flood are repeatedly kicked into the qualitative discriminating of row.
Particularly, the qualitative discriminating of emblic comprises:
1a) prepare emblic need testing solution, emblic control medicinal material solution, not containing the negative sample solution of emblic;
2a) according to 2010 editions appendix VIB tests of thin-layered chromatography < < Chinese Pharmacopoeia > >, 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) take petroleum ether-ethyl acetate-formic acid that boiling point is 60～90 ℃ is developping agent, by step 2a) thin layer plate that obtains be placed on saturated in expansion cylinder, launch, take out, dry, spray is with liquor ferri trichloridi, wind is clear to spot colour developing; In thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram;
The qualitative discriminating of Hong Lian comprises:
1b) preparation flood connects need testing solution, the big vast negative sample solution that connects control medicinal material solution, do not connect containing flood;
2b) according to 2010 editions appendix VIB tests of thin-layered chromatography < < Chinese Pharmacopoeia > >, 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) take methyl alcohol-acetic acid-water 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, connecting on the corresponding position of control medicinal material chromatogram the spot of the aobvious same color of test sample chromatogram with flood.
The preparation method of the need testing solution that particularly, described emblic, flood connect, control medicinal material solution, negative sample solution comprises:
(1) need testing solution of emblic, control medicinal material solution, negative sample solution
Get described Six-element caragana preparation, porphyrize, adds methyl alcohol, and ultrasonic processing filters, and filtrate is concentrated, as emblic need testing solution; Separately get emblic control medicinal material, according to the preparation method of described emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of described emblic need testing solution;
(2) flood connects need testing solution, control medicinal material solution, negative sample solution
Get described Six-element caragana preparation, porphyrize, adds methyl alcohol, and ultrasonic processing filters, and filtrate is concentrated, as flood, connects need testing solution; Separately get flood and connect control medicinal material, the preparation method who connects need testing solution according to described flood makes flood and connects control medicinal material solution; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by described flood is made even negative sample solution of flood.
More specifically, described detection method comprises the following steps:
A) the qualitative discriminating of emblic
Get described Six-element caragana preparation 0.5～5 weight portion, porphyrize, adds methyl alcohol 5～40 parts by volume, and ultrasonic processing 10～60 minutes filters, and filtrate is concentrated into 0.5～8 parts by volume, as emblic need testing solution; Separately get emblic control medicinal material 0.1～2.5 weight portion, according to the preparation method of described emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of described emblic need testing solution.According to thin-layered chromatography test described in appendix VIB of < < Chinese Pharmacopoeia > > version in 2010, draw each 0.001～0.02 parts by volume of above-mentioned three kinds of solution, point sample is on same silica gel g thin-layer plate respectively, petroleum ether-ethyl acetate-formic acid that the boiling point of take is 60～90 ℃ is developping agent, the volume ratio of developping agent is petroleum ether-ethyl acetate-formic acid (1～15: 1～9: 0.05～0.5), thin layer plate is put in expansion cylinder saturated 0～40 minute, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast, in thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram,
B) the qualitative discriminating that flood connects
Get described Six-element caragana preparation 0.5～5 weight portion, porphyrize, adds acetone 5～40 parts by volume, and ultrasonic processing 10～60 minutes filters, and filtrate is concentrated into 0.5～8 parts by volume, as flood, connects need testing solution; Separately get flood and connect control medicinal material 0.1～2.5 weight portion, the preparation method who connects need testing solution according to described flood makes flood and connects control medicinal material solution; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by described flood is made even negative sample solution of flood; According to thin-layered chromatography test described in appendix VIB of < < Chinese Pharmacopoeia > > version in 2010, draw each 0.001～0.02 parts by volume of above-mentioned three kinds of solution, put respectively on same polyamide film, take volume ratio as 0.1～10: methyl alcohol-acetic acid-water of 0.05～5: 1～20 is developping agent, thin layer plate is put in expansion cylinder saturated 0～40 minute, launches, and takes out, dry, put under 365nm ultraviolet lamp and inspect; In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram the spot of the aobvious same color of test sample chromatogram with flood.
More specifically, described detection method comprises the following steps:
I) the qualitative discriminating of emblic:
Get described Six-element caragana preparation 2g, porphyrize, adds methyl alcohol 20ml, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4ml, as emblic need testing solution, separately get emblic control medicinal material 0.5g, according to the preparation method of described emblic need testing solution, make emblic control medicinal material solution, in prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of described emblic need testing solution, according to thin-layered chromatography test described in appendix VIB of < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ L of above-mentioned three kinds of solution, point sample is on same silica gel g thin-layer plate respectively, petroleum ether-ethyl acetate-formic acid that the boiling point of take is 60～90 ℃ is developping agent, the volume ratio of developping agent is petroleum ether-ethyl acetate-formic acid (6: 4: 0.25), thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast, in thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram,
Ii) the qualitative discriminating that flood connects
Get described Six-element caragana preparation 2g, porphyrize, adds acetone 20ml, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4ml, as flood, connects need testing solution; Separately get flood and connect control medicinal material 0.5g, the preparation method who connects need testing solution according to described flood makes flood and connects control medicinal material solution; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by described flood is made even negative sample solution of flood; According to thin-layered chromatography test described in appendix VIB of < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ L of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-water that the volume ratio of take is 2: 1: 7 is developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, put under 365nm ultraviolet lamp and inspect; In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram the spot of the aobvious same color of test sample chromatogram with flood.
The formulation of Six-element caragana preparation of the present invention can be tablet, capsule, granule, pill or powder.Preparation method is: get described Six-element caragana preparation, be ground into fine powder, sieve, mix, add suitable quantity of water pill, dry in the shade and get final product; Or get described Six-element caragana preparation, and be ground into fine powder, sieve, mix, by pharmacy conventional method, add conventional auxiliary material, make the oral formulations of accepting clinically: granule, pill, capsule, tablet or powder.
The present invention is directed to the constituent of Six-element caragana preparation, index composition emblic, flood are repeatedly kicked into row qualitative detection, to reach the object that the quality of preparation is controlled.The invention provides the detection method of good Six-element caragana preparation, that this detection method has is sensitive, favorable reproducibility and the strong feature of specificity.
Accompanying drawing explanation
Fig. 1 is emblic thin-layer chromatography discriminating figure in Six-element caragana preparation;
Wherein sample is sequentially from left to right: need testing solution 1, need testing solution 2, need testing solution 3, emblic control medicinal material solution, emblic control medicinal material solution, emblic negative sample solution;
Wherein developping agent is sherwood oil (60 ℃～90 ℃)-ethyl acetate-formic acid (6: 4: 0.25).
Fig. 2 is that in Six-element caragana preparation, flood connects thin-layer chromatography discriminating figure;
Wherein sample is sequentially from left to right: need testing solution 1, need testing solution 2, need testing solution 3, flood connect control medicinal material solution, flood connects control medicinal material solution, the big vast negative sample solution that connects;
Wherein developping agent is methyl alcohol-acetic acid-water (2: 1: 7).
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 is the test sample of preparing according to each discrimination method requirement, for example, at the test sample described in the qualitative discrimination method of emblic, be " test sample of the qualitative discriminating of emblic ".
Experimental example 1: the screening experiment of the thin-layer chromatography condition of emblic
(1) instrument
Electronic scales, tool plug conical flask, transfer pipet, ultrasound wave extraction apparatus, funnel, filter paper, evaporating dish, sample applicator, silica G plate, chromatography cylinder, spray bottle, hair dryer.
(2) control medicinal material
Emblic control medicinal material (lot number: 121289-200301), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
(3) reagent
Methyl alcohol, ether, acetone, sherwood oil (60～90 ℃), ethyl acetate, formic acid, ferric trichloride.
(4) method of inspection
Extract the selection of solvent: adopt respectively the solution such as ether, acetone, methyl alcohol for extracting solvent;
The selection of extracting method: adopt respectively ultrasonic extraction and cold soaking to extract;
The selection of developping agent: adopting respectively sherwood oil (60～90 ℃)-ethyl acetate (3: 8), sherwood oil (60～90 ℃)-ethyl acetate (6: 4), sherwood oil (60～90 ℃)-ethyl acetate-formic acid (6: 4: 0.25) is developping agent;
Select respectively above solvent, extracting method and the developping agent of extracting to test, result is as follows:
Repetition test in the above conditions, finally determined that the specificity thin-layer identification method of emblic is as follows:
Prepare first group of sample solution, get described Six-element caragana preparation 2g, porphyrize, adds methyl alcohol 20mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4mL, as emblic need testing solution; Separately get emblic control medicinal material 0.5g, according to the preparation method of emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of above-mentioned emblic need testing solution; According to appendix VI B test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, sherwood oil (60～90 ℃)-ethyl acetate-formic acid (6: 4: 0.25) of take are developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast.As shown in Figure 1, in thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
Experimental example 2: the screening experiment of the thin-layer chromatography condition that flood connects
(1) instrument
Electronic scales, tool plug conical flask, transfer pipet, ultrasound wave extraction apparatus, funnel, filter paper, evaporating dish, sample applicator, polyamide film, chromatography cylinder.
(2) control medicinal material
Big vast even control medicinal material (lot number: 121242-200401), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
(3) reagent
Methyl alcohol, ethyl acetate, ether, acetic acid, water.
(4) method of inspection:
Extract the selection of solvent: adopt respectively the solution such as methyl alcohol, ethyl acetate, ether for extracting solvent;
The selection of extracting method: adopt respectively ultrasonic extraction and cold soaking to extract;
The selection of developping agent: adopting respectively methanol-water (2: 7), methyl alcohol-acetic acid-water (2: 1: 7) is developping agent;
Select respectively above solvent, extracting method and the developping agent of extracting to test, result is as follows:
Repetition test in the above conditions, finally determined that the specificity thin-layer identification method of big vast company is as follows:
Prepare second group of sample solution, get described Six-element caragana preparation 2g, porphyrize, adds methyl alcohol 20mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4mL, as flood, connects need testing solution; Separately get flood and connect control medicinal material 0.5g, the preparation method who connects need testing solution according to flood makes even control medicinal material solution of flood; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by above-mentioned flood is made even negative sample solution of flood; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-the water (2: 1: 7) of take is developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launches, and takes out, dry, put under ultraviolet lamp (365nm) and inspect.As shown in Figure 2, in thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram with flood, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
Following embodiment all can realize the effect of above-mentioned experimental example.
The preparation of [embodiment 1] Six-element caragana preparation
The cream 100g such as ZANGJINJIER/shagspine peashrub bark stem and leaf 150g, BAXIAGA 100g, emblic 130g, Herba Corydalis 100g, Song Sheng, flood are connected to 100g, be ground into fine powder, sieve, mix, add suitable quantity of water pill, dry in the shade and get final product; Or get above Six-element, and be ground into fine powder, sieve, mix, by pharmacy conventional method, add conventional auxiliary material, make the oral formulations of accepting clinically: granule, pill, capsule, tablet or powder.
Usage and the consumption of described Six-element caragana preparation: a day dose is 2g crude drug amount, 2 times on the one.
[embodiment 2] discriminating that Six-element caragana soup is loose
The cream 100g such as ZANGJINJIER/shagspine peashrub bark stem and leaf 150g, BAXIAGA 100g, emblic 130g, Herba Corydalis 100g, Song Sheng, flood connect 100g;
Above Six-element, is ground into fine powder, sieves, and mixes, and obtains.
A. the thin layer of emblic is differentiated
Get the loose 2g of described Six-element caragana soup, add methyl alcohol 20mL, ultrasonic processing 30 minutes, filters, and filtrate is concentrated into 4mL, as emblic need testing solution.Separately get emblic control medicinal material 0.5g, according to the preparation method of emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of above-mentioned emblic need testing solution; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, sherwood oil (60～90 ℃)-ethyl acetate-formic acid (6: 4: 0.25) of take are developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast.In thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
B. the thin layer that flood connects is differentiated
Get the loose 2g of described Six-element caragana soup, add methyl alcohol 20mL, ultrasonic processing 30 minutes, filters, and filtrate is concentrated into 4mL, as flood, connects need testing solution.Separately get flood and connect control medicinal material 0.5g, the preparation method who connects need testing solution according to flood makes even control medicinal material solution of flood; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by above-mentioned flood is made even negative sample solution of flood; According to appendix VI B test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-the water (2: 1: 7) of take is developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launches, and takes out, dry, put under ultraviolet lamp (365nm) and inspect.In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram with flood, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
The discriminating of [embodiment 3] Six-element caragana particle
The cream 80g such as ZANGJINJIER/shagspine peashrub bark stem and leaf 120g, BAXIAGA 80g, emblic 100g, Herba Corydalis 80g, Song Sheng, flood connect 80g;
Above Six-element, is ground into fine powder, sieves, and mixes, and by pharmacy conventional method, adds conventional auxiliary material, makes the Six-element caragana particle of accepting clinically.
A. the thin layer of emblic is differentiated
Get described Six-element caragana particle 0.5g, porphyrize, adds methyl alcohol 5mL, and ultrasonic processing 15 minutes filters, and filtrate is concentrated into 1mL, as emblic need testing solution.Separately get emblic control medicinal material 0.2g, according to the preparation method of emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of above-mentioned emblic need testing solution; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, sherwood oil (60～90 ℃)-ethyl acetate-formic acid (2: 1.6: 0.1) of take are developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast.In thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
B. the thin layer that flood connects is differentiated
Get described Six-element caragana particle 0.5g, porphyrize, adds methyl alcohol 5mL, and ultrasonic processing 15 minutes filters, and filtrate is concentrated into 1mL, as flood, connects need testing solution.Separately get flood and connect control medicinal material 0.2g, the preparation method who connects need testing solution according to flood makes even control medicinal material solution of flood; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by above-mentioned flood is made even negative sample solution of flood; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-the water (0.5: 0.3: 1.8) of take is developping agent, thin layer plate is put in expansion cylinder saturated 30 minutes, launches, and takes out, dry, put under ultraviolet lamp (365nm) and inspect.In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram with flood, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
The discriminating of [embodiment 4] Six-element caragana ball
The cream 120g such as ZANGJINJIER/shagspine peashrub bark stem and leaf 180g, BAXIAGA 120g, emblic 150g, Herba Corydalis 120g, Song Sheng, flood connect 120g;
Above Six-element, is ground into fine powder, sieves, and mixes, and by pharmacy conventional method, adds conventional auxiliary material, makes the Six-element caragana ball of accepting clinically.
A. the thin layer of emblic is differentiated
Get described Six-element caragana ball 4.5g, porphyrize, adds methyl alcohol 40mL, and ultrasonic processing 45 minutes filters, and filtrate is concentrated into 2mL, as emblic need testing solution.Separately get emblic control medicinal material 1g, according to the preparation method of emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of above-mentioned emblic need testing solution; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, sherwood oil (60～90 ℃)-ethyl acetate-formic acid (10: 6: 0.2) of take are developping agent, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast.In thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
B. the thin layer that flood connects is differentiated
Get described Six-element caragana ball 4.5g, porphyrize, adds methyl alcohol 40mL, and ultrasonic processing 45 minutes filters, and filtrate is concentrated into 2mL, as flood, connects need testing solution.Separately get flood and connect control medicinal material 1g, the preparation method who connects need testing solution according to flood makes even control medicinal material solution of flood; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by above-mentioned flood is made even negative sample solution of flood; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-the water (4: 3: 10) of take is developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launches, and takes out, dry, put under ultraviolet lamp (365nm) and inspect.In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram with flood, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
The discriminating of [embodiment 5] Six-element caragana hard shell capsules
The cream 100g such as ZANGJINJIER/shagspine peashrub bark stem and leaf 150g, BAXIAGA 100g, emblic 130g, Herba Corydalis 100g, Song Sheng, flood connect 100g;
Above Six-element, is ground into fine powder, sieves, and mixes, and by pharmacy conventional method, adds conventional auxiliary material, makes the Six-element caragana hard shell capsules of accepting clinically.
A. the thin layer of emblic is differentiated
Get described Six-element caragana hard shell capsules 2g, porphyrize, adds methyl alcohol 20mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4mL, as emblic need testing solution.Separately get emblic control medicinal material 0.5g, according to the preparation method of emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of above-mentioned emblic need testing solution; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, sherwood oil (60～90 ℃)-ethyl acetate-formic acid (6: 4: 0.25) of take are developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast.In thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
B. the thin layer that flood connects is differentiated
Get described Six-element caragana hard shell capsules 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 20 minutes filters, and filtrate is concentrated into 5mL, as flood, connects need testing solution.Separately get flood and connect control medicinal material 1.5g, the preparation method who connects need testing solution according to flood makes even control medicinal material solution of flood; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by above-mentioned flood is made even negative sample solution of flood; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 15 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-the water (6: 4.6: 12) of take is developping agent, launch, take out, dry, put under ultraviolet lamp (365nm) and inspect.In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram with flood, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
The discriminating of [embodiment 6] Six-element caragana sheet
The cream 80g such as ZANGJINJIER/shagspine peashrub bark stem and leaf 120g, BAXIAGA 120g, emblic 100g, Herba Corydalis 120g, Song Sheng, flood connect 120g;
Above Six-element, is ground into fine powder, sieves, and mixes, and by pharmacy conventional method, adds conventional auxiliary material, makes the Six-element caragana sheet of accepting clinically.
A. the thin layer of emblic is differentiated
Get described Six-element caragana sheet 1g, porphyrize, adds methyl alcohol 10mL, and ultrasonic processing 20 minutes filters, and filtrate is concentrated into 5mL, as emblic need testing solution.Separately get emblic control medicinal material 1.5g, according to the preparation method of emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of above-mentioned emblic need testing solution; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 15 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, sherwood oil (60～90 ℃)-ethyl acetate-formic acid (12: 6.5: 0.3) of take are developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast.In thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
B. the thin layer that flood connects is differentiated
Get described Six-element caragana sheet 2g, porphyrize, adds methyl alcohol 20mL, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4mL, as flood, connects need testing solution.Separately get flood and connect control medicinal material 0.5g, the preparation method who connects need testing solution according to flood makes even control medicinal material solution of flood; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by above-mentioned flood is made even negative sample solution of flood; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-the water (2: 1: 7) of take is developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launches, and takes out, dry, put under ultraviolet lamp (365nm) and inspect.In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram with flood, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
The discriminating of [embodiment 7] Six-element caragana soft capsule
The cream 120g such as ZANGJINJIER/shagspine peashrub bark stem and leaf 180g, BAXIAGA 80g, emblic 150g, Herba Corydalis 80g, Song Sheng, flood connect 80g;
Above Six-element, is ground into fine powder, sieves, and mixes, and by pharmacy conventional method, adds conventional auxiliary material, makes the Six-element caragana soft capsule of accepting clinically.
A. the thin layer of emblic is differentiated
Get described Six-element caragana soft capsule 3.5g, add methyl alcohol 30mL, ultrasonic processing 60 minutes, filters, and filtrate is concentrated into 6mL, as emblic need testing solution.Separately get emblic control medicinal material 2g, according to the preparation method of emblic need testing solution, make emblic control medicinal material solution; In prescription ratio and preparation technology, configuration does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of above-mentioned emblic need testing solution; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, sherwood oil (60～90 ℃)-ethyl acetate-formic acid (14: 8: 0.4) of take are developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast.In thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
B. the thin layer that flood connects is differentiated
Get described Six-element caragana soft capsule 3.5g, add methyl alcohol 30mL, ultrasonic processing 60 minutes, filters, and filtrate is concentrated into 6mL, as flood, connects need testing solution.Separately get flood and connect control medicinal material 2g, the preparation method who connects need testing solution according to flood makes even control medicinal material solution of flood; In prescription ratio and preparation technology, configuration is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by above-mentioned flood is made even negative sample solution of flood; According to appendix VIB test of thin-layered chromatography < < Chinese Pharmacopoeia > > version in 2010, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-the water (8.4: 3.8: 6.5) of take is developping agent, thin layer plate is put in expansion cylinder saturated 40 minutes, launches, and takes out, dry, put under ultraviolet lamp (365nm) and inspect.In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram with flood, the spot of the aobvious same color of test sample chromatogram, and negative noiseless.
Claims (3)
1. a detection method for Six-element caragana preparation, described preparation raw material medicine consists of: cream 100 weight portions such as ZANGJINJIER/shagspine peashrub bark stem and leaf 150 weight portions, BAXIAGA 100 weight portions, emblic 130 weight portions, Herba Corydalis 100 weight portions, Song Sheng, flood connect 100 weight portions;
Described detection method, comprises the following steps: i) the qualitative discriminating of emblic:
Get described Six-element caragana preparation 2g, porphyrize, adds methyl alcohol 20ml, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4ml, as emblic need testing solution, separately get emblic control medicinal material 0.5g, according to the preparation method of described emblic need testing solution, make emblic control medicinal material solution, in prescription ratio and preparation technology, preparation does not contain the negative sample of emblic, and makes emblic negative sample solution by the compound method of described emblic need testing solution, according to thin-layered chromatography test described in appendix VI B of < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ L of above-mentioned three kinds of solution, point sample is on same silica gel g thin-layer plate respectively, petroleum ether-ethyl acetate-formic acid that the boiling point of take is 60～90 ℃ is developping agent, the volume ratio of developping agent is petroleum ether-ethyl acetate-formic acid=6:4:0.25, thin layer plate is put in expansion cylinder saturated 20 minutes, launch, take out, dry, it is clear that spray is blown to spot colour developing with 10% liquor ferri trichloridi hot blast, in thin-layer chromatography, with the corresponding position of emblic control medicinal material chromatogram on, the spot of the aobvious same color of test sample chromatogram,
Ii) the qualitative discriminating that flood connects
Get described Six-element caragana preparation 2g, porphyrize, adds methyl alcohol 20ml, and ultrasonic processing 30 minutes filters, and filtrate is concentrated into 4ml, as flood, connects need testing solution; Separately get flood and connect control medicinal material 0.5g, according to described flood, connect the preparation method of need testing solution, make flood and connect control medicinal material solution; In prescription ratio and preparation technology, preparation is not containing the big vast negative sample connecting, and the compound method that connects need testing solution by described flood is made even negative sample solution of flood; According to thin-layered chromatography test described in appendix VI B of < < Chinese Pharmacopoeia > > version in 2010, draw each 5 μ L of above-mentioned three kinds of solution, put respectively on same polyamide film, methyl alcohol-acetic acid-water that the volume ratio of take is 2:1:7 is developping agent, thin layer plate is put in expansion cylinder saturated 20 minutes, launches, and takes out, dry, put under 365nm ultraviolet lamp and inspect; In thin-layer chromatography, connecting on the corresponding position of control medicinal material chromatogram the spot of the aobvious same color of test sample chromatogram with flood.
2. detection method as claimed in claim 1, is characterized in that, the formulation of described Six-element caragana preparation is tablet, capsule, granule, pill or powder.
3. detection method as claimed in claim 1, is characterized in that, gets described Six-element caragana preparation, 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 Six-element caragana preparation, 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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