CN104297413B - The method of inspection of acrobatic fighting general's tincture - Google Patents
The method of inspection of acrobatic fighting general's tincture Download PDFInfo
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- CN104297413B CN104297413B CN201410527271.2A CN201410527271A CN104297413B CN 104297413 B CN104297413 B CN 104297413B CN 201410527271 A CN201410527271 A CN 201410527271A CN 104297413 B CN104297413 B CN 104297413B
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Abstract
The invention discloses a kind of method of inspection of acrobatic fighting general tincture, on the basis of the existing giant knotweed of discriminating respectively of acrobatic fighting general's Quality of Liquors standard, Ligusticum wallichii, paniculate swallowwort, menthol, Resina Draconis, the thin layer for improving Ligusticum wallichii differentiates, the thin layer that increased curcuma zedoary differentiates, is improved to silica gel H adsorbent by the silica G adsorbent for differentiating primary standard, by ethyl acetate hexane (9:1) solvent is improved to petroleum ether (30 60 DEG C) ethyl acetate (98:2), it is achieved that under the conditions of same thin-layer chromatography, by different inspection methods, while differentiating two taste medicinal material of Ligusticum wallichii and curcuma zedoary；Meanwhile, the assay to giant knotweed and paniculate swallowwort medicine is increased, i.e.,：Using the content of the active ingredient Paeonol of the content and paniculate swallowwort of the active ingredient polygonin of giant knotweed in high effective liquid chromatography for measuring acrobatic fighting general's tincture finished product, so as to improve the specificity and validity of Drug's control, the effective control to acrobatic fighting general's tincture product quality is advantageously implemented.
Description
Technical field
A kind of the invention belongs to drug quality detection technique field, more particularly to method of inspection of acrobatic fighting general tincture.
Background technology
Acrobatic fighting general's tincture be one kind be widely used in treating traumatic injury, muscles and bones sprain, treating rheumatic ostealgia, rheumatoid arthrosis
Bitterly, the strong medicine preparation of osteoproliferation shouting pain, it come from same prescription with " acrobatic fighting general's wine ", by toddalia, mountain spicy tree root and rhizome,
The 13 taste medicinal material such as Resina Draconis is made.The quality standard of the series of products " acrobatic fighting general's wine " is recorded and defends medicine pharmacy word in osmanthus
(2003) 800005, the thin-layer identification method for having giant knotweed, Ligusticum wallichii, paniculate swallowwort, menthol, Resina Draconis is only worked out, quantitative without medicine
Detection, is unfavorable for the quality good or not of effective control finished product.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of method of inspection of accurately and reliably acrobatic fighting general's tincture, to meet
The needs of acrobatic fighting general's tincture control of product quality.
For solving above-mentioned technical problem, the present invention is employed the following technical solutions：The method of inspection of acrobatic fighting general's tincture, including river
The assay of the thin layer discriminating, giant knotweed and paniculate swallowwort of rhizome of chuanxiong and curcuma zedoary；Thin layer differentiates to adopt volume ratio for 98:2 petroleum ether
(30-60 DEG C)-ethyl acetate mixtures are solvent, first put, then spray with 5% after expansion
Phosphomolybdic acid test solution, heating inspect curcuma zedoary under daylight；Assay is using polygonin in high effective liquid chromatography for measuring giant knotweed
With the content of Paeonol in paniculate swallowwort, high performance liquid chromatography with octadecylsilane chemically bonded silica as filler, respectively with first
Alcohol and water is that mobile phase A and Mobile phase B carry out gradient elution.
The method of inspection of above-mentioned acrobatic fighting general tincture, according to the following steps operation are carried out：
<1>The thin layer of Ligusticum wallichii and curcuma zedoary differentiates
This product 30ml is taken, is put in separatory funnel, add water 30ml, shakes up, the shaking that adds diethyl ether is extracted 2 times, each 30ml merges
Ether solution, plus anhydrous sodium sulfate 10g, shaking, filtration, filtrate are volatilized, and residue adds methyl alcohol 2ml to make dissolving, used as need testing solution；
Ligusticum wallichii control medicinal material powder 1g is taken, add diethyl ether 20ml, 40 DEG C of heating water baths flow back 1 hour, and filtration, filtrate are volatilized, and residue adds second
Acetoacetic ester 2ml makes dissolving, used as control medicinal material solution；Take germacrone reference substance again, plus absolute ethyl alcohol is made every ml and contains 0.4mg's
Solution, used as reference substance solution；Test with reference to Chinese Pharmacopoeia (the one annex VIB of version in 2010) thin-layered chromatography, draw above-mentioned
Each 8～10 μ 1 of three kinds of solution, is put respectively on same silica gel H lamellae, with volume ratio as 98:2 petroleum ether (30-60 DEG C)-
Ethyl acetate mixtures are solvent, launch, take out, dry, put, in test sample chromatogram, with
On the corresponding position of control medicinal material chromatogram, show the main fluorescence spot of same color；Sprayed with 5% phosphomolybdic acid test solution again, hot blast is blown to
Clear spot, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows the spot of same color；
<2>In giant knotweed in polygonin and paniculate swallowwort Paeonol assay
Carry out with reference to the operation of Chinese Pharmacopoeia (the one annex VI D of version in 2010) liquid chromatography：
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methyl alcohol as mobile phase
A, with water as Mobile phase B, the regulation according to the form below carries out gradient elution；Variable-wavelength measure；Number of theoretical plate is based on polygonin peak
5000 should be not less than；3000 should be not less than based on Paeonol peak；
The preparation of reference substance solution takes polygonin reference substance with Paeonol reference substance in right amount, accurately weighed, plus methyl alcohol is made
Mixed solution in per ml containing 20 μ g of 40 μ g of polygonin and Paeonol, obtains final product；
The preparation precision of need testing solution measures this product 1ml, puts in 10ml measuring bottles, plus methanol dilution is to scale, shakes up, filter
Cross, subsequent filtrate is taken as need testing solution；
Determination method is accurate respectively to draw reference substance and each 10 μ l of need testing solution, injects liquid chromatograph, determines, obtain final product.
Above-mentioned acrobatic fighting general tincture is prepared according to the following steps：Take giant knotweed 150g, curcuma zedoary 100g, paniculate swallowwort 50g, Ligusticum wallichii 50g, fly
Dragon palm blood 50g, Bi roots of grass 50g, rhizome of davallia 50g, frankincense 6g, pseudo-ginseng 6g, Resina Draconis 1g, mountain spicy tree root and rhizome 50g, saltcake 10g, menthol 4g
Totally ten three taste, in addition to frankincense, saltcake, Resina Draconis, menthol, pseudo-ginseng is individually ground into eight tastes such as most meal, remaining giant knotweed also together
Most meal is ground into, is put in container, add 50% ethanol 1800ml, closed, impregnate 40 days；Filtration, filtrate are standby；Frankincense, awns
Nitre, Resina Draconis are ground respectively, are added in above-mentioned filtrate, are stirred evenly, closed, stand 15 days；Supernatant is taken, menthol, stirring is added
Dissolving is made, plus 50% ethanol is 1000ml to total amount, stirs evenly, obtains final product.
Most meal refers to the medicinal powder that can cross a sieve (Chinese Pharmacopoeia screen size).
Formula Development acrobatic fighting general tincture of the inventor according to hot-sale products acrobatic fighting general's wine, right proper mass standard only have tiger
Cane, paniculate swallowwort, Ligusticum wallichii, menthol, the discriminating of Resina Draconis-drug thin layer, still lack Qualitive test and main ingredient giant knotweed and Xu of main ingredient curcuma zedoary
The assay of long minister in ancient times, it is difficult to realize the good and bad effective control to acrobatic fighting general's tincture drug quality.For this purpose, in proper mass standard
On the basis of the giant knotweed of discriminating respectively that has, Ligusticum wallichii, paniculate swallowwort, menthol, Resina Draconis, inventor improves the thin layer mirror of Ligusticum wallichii
, not increased curcuma zedoary thin layer differentiate, by the silica G adsorbent that primary standard is differentiated be improved to silica gel H adsorbent, will just oneself
Alkane-ethyl acetate (9:1) solvent is improved to petroleum ether (30-60 DEG C)-ethyl acetate (98:2), it is achieved that in same thin layer color
Under spectral condition, by different inspection methods, two taste medicinal material of Ligusticum wallichii and curcuma zedoary can be differentiated simultaneously；Meanwhile, invention increases right
Giant knotweed and the assay of paniculate swallowwort medicine, i.e.,：Had using giant knotweed in high effective liquid chromatography for measuring acrobatic fighting general's tincture finished product
The content of the active ingredient Paeonol of the content and paniculate swallowwort of effect composition polygonin, so that improve the exclusive of Drug's control
Property and validity, are advantageously implemented the effective control to acrobatic fighting general's tincture product quality.
Specific embodiment
Following examples agents useful for same and equipment are as follows：
1. germacrone reference substance：Lot number：111665-201204, National Institute for Food and Drugs Control are provided.
2. Ligusticum wallichii control medicinal material：Lot number：120918-201110, National Institute for Food and Drugs Control are provided.
3. Paeonol reference substance：Lot number：110708-200506, National Institute for Food and Drugs Control are provided.
4. polygonin reference substance：Lot number：11575-200502, National Institute for Food and Drugs Control are provided.
5. test specimen：The homemade acrobatic fighting general tincture of applicant and acrobatic fighting general's wine.
6. Shimadzu LC-20A high performance liquid chromatograph, PDAD, LC Solution chromatographic work station (days
This Shimadzu Corporation).
7.YOKO-ZS ultra-violet analysis photographic apparatus (Wuhan medicine new technology development Co., Ltd).
8.1/105Electronic analytical balance XS205BDU (Mei Tele companies of Switzerland).
Embodiment 1 prepares acrobatic fighting general's tincture
Take giant knotweed 150g, curcuma zedoary 100g, paniculate swallowwort 50g, Ligusticum wallichii 50g, toddalia 50g, Bi roots of grass 50g, rhizome of davallia 50g,
Frankincense 6g, pseudo-ginseng 6g, Resina Draconis 1g, mountain spicy tree root and rhizome 50g, saltcake 10g, menthol 4g totally ten three taste, except frankincense, saltcake, Resina Draconis,
Outside menthol, pseudo-ginseng is individually ground into most meal (crossing a pharmacopeia sieve), and eight taste such as remaining giant knotweed is also ground into most meal together, puts
In container, 50% ethanol 1800ml is added, closed, impregnate 40 days；Filtration, filtrate are standby；Frankincense, saltcake, Resina Draconis are ground respectively
Broken, add in above-mentioned filtrate, stir evenly, closed, stand 15 days；Supernatant is taken, menthol is added, is stirred to dissolve, plus 50% second
Alcohol is 1000ml to total amount, stirs evenly, obtains final product.
Three batches of acrobatic fighting general's tincture products are prepared according to said method, lot number is respectively 140501,140502,140503.
The thin layer of 2 Ligusticum wallichii of embodiment and curcuma zedoary differentiates
Three batch acrobatic fighting general's tincture products of Example 1, the method for inspection that sets up by the present invention carry out Ligusticum wallichii and curcuma zedoary
Thin layer differentiate, specific as follows：
This product 30ml is taken, is put in separatory funnel, add water 30ml, shakes up, the shaking that adds diethyl ether is extracted 2 times, each 30ml merges
Ether solution, plus anhydrous sodium sulfate 10g, shaking, filtration, filtrate are volatilized, and residue adds methyl alcohol 2ml to make dissolving, used as need testing solution；
Ligusticum wallichii control medicinal material powder 1g is taken, add diethyl ether 20ml, 40 DEG C of heating water baths flow back 1 hour, and filtration, filtrate are volatilized, and residue adds second
Acetoacetic ester 2ml makes dissolving, used as control medicinal material solution；Take germacrone reference substance again, plus absolute ethyl alcohol is made every ml and contains 0.4mg's
Solution, used as reference substance solution；With reference to Chinese Pharmacopoeia thin-layered chromatography (Chinese Pharmacopoeia one VI B of annex of version in 2010) test,
Each 8～10 μ 1 of above-mentioned three kinds of solution is drawn, is put on same silica gel H lamellae, with volume ratio as 98 respectively:2 petroleum ether
(30-60 DEG C)-ethyl acetate mixtures are solvent, launch, and take out, dry, put.Test sample
In chromatogram, on position corresponding with Ligusticum wallichii control medicinal material chromatogram, show the main fluorescence spot of same color；Sprayed with 5% phosphorus molybdenum again
Sour test solution, is heated to clear spot；In test sample chromatogram, on position corresponding with reference substance chromatogram, show identical bluish violet
Spot.
In 3 giant knotweed of embodiment in polygonin and paniculate swallowwort Paeonol assay
Three batch acrobatic fighting general's tincture products of Example 1, the method for inspection that sets up by the present invention carry out giant knotweed in giant knotweed
In glycosides and paniculate swallowwort, the assay of Paeonol, specific as follows：
Carry out with reference to liquid chromatography (Chinese Pharmacopoeia one VI D of annex of version in 2010) operation：
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methyl alcohol as mobile phase
A, with water as Mobile phase B, the regulation according to the form below carries out gradient elution；Variable-wavelength measure；Flow velocity is 0.8ml per minute；Reason
5000 should be not less than based on polygonin peak by plate number；3000 should be not less than based on Paeonol peak；
The preparation of reference substance solution takes polygonin reference substance with Paeonol reference substance in right amount, accurately weighed, plus methyl alcohol is made
Mixed solution in per ml containing 20 μ g of 40 μ g of polygonin and Paeonol, obtains final product；
The preparation precision of need testing solution measures this product 1ml, puts in 10ml measuring bottles, plus methanol dilution is to scale, shakes up,
Filtration, takes subsequent filtrate as need testing solution；
Determination method is accurate respectively to draw reference substance and each 10 μ l of need testing solution, injects liquid chromatograph, determines, obtain final product.
Three batch acrobatic fighting general's wine products are taken, and [medicine pharmacy word (2003) are defended in osmanthus with reference to acrobatic fighting general's Quality of Liquors standard
800005] test, embodiment and contrast and experiment are as follows.
1 acrobatic fighting general wine of table and acrobatic fighting general's tincture qualitative, quantitative measurement result
By the method for inspection of the present invention, acrobatic fighting general tincture is per 1ml containing giant knotweed with polygonin (C20H22O8) must not count and be less than
0.05mg；Per 1ml containing paniculate swallowwort with Paeonol (C9H10O3) must not count less than 0.06mg.
Claims (3)
1. a kind of method of inspection of acrobatic fighting general tincture, it is characterised in that including Ligusticum wallichii and curcuma zedoary thin layer differentiate, giant knotweed and Xu long
The assay of minister in ancient times；The thin layer differentiates that it is solvent for 98: 2 petroleum ether-ethyl acetate mixed liquor to adopt volume ratio, launches
First put afterwards, then spray with 5% phosphomolybdic acid test solution, heating inspects curcuma zedoary under daylight；Described
Content of the assay using Paeonol in polygonin in high effective liquid chromatography for measuring giant knotweed and paniculate swallowwort, high performance liquid chromatography
Method is carried out gradient and is washed with first alcohol and water as mobile phase A with Mobile phase B respectively with octadecylsilane chemically bonded silica as filler
De-；Specifically operation is carried out the method according to the following steps：
<1>The thin layer of Ligusticum wallichii and curcuma zedoary differentiates
This product 30ml is taken, is put in separatory funnel, add water 30ml, shakes up, the shaking that adds diethyl ether is extracted 2 times, each 30ml merges ether
Liquid, plus anhydrous sodium sulfate 10g, shaking, filtration, filtrate are volatilized, and residue adds methyl alcohol 2ml to make dissolving, used as need testing solution；Take river
Rhizome of chuanxiong control medicinal material powder 1g, add diethyl ether 20ml, and 40 DEG C of heating water baths flow back 1 hour, and filtration, filtrate are volatilized, and residue adds acetic acid second
Ester 2ml makes dissolving, used as control medicinal material solution；Take germacrone reference substance again, plus absolute ethyl alcohol is made every ml and contains the molten of 0.4mg
Liquid, used as reference substance solution；With reference to Chinese Pharmacopoeia one annex VI B thin-layered chromatography test of version in 2010, draw above-mentioned three kinds
Each 8～10 μ l of solution, are put on same silica gel H lamellae respectively, the petroleum ether-ethyl acetate mixed liquor with volume ratio as 98: 2
For solvent, launch, take out, dry, put, in test sample chromatogram, with control medicinal material chromatogram phase
On the position that answers, show the main fluorescence spot of same color；Sprayed with 5% phosphomolybdic acid test solution again, hot blast is blown to clear spot, test sample
In chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color；
<2>In giant knotweed in polygonin and paniculate swallowwort Paeonol assay
Carry out with reference to Chinese Pharmacopoeia one annex VI D liquid chromatography operation of version in 2010：
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methyl alcohol as mobile phase A, with
Water is Mobile phase B, and the regulation according to the form below carries out gradient elution；Variable-wavelength measure；Number of theoretical plate should not based on polygonin peak
It is less than 5000；3000 should be not less than based on Paeonol peak；
The preparation of reference substance solution takes polygonin reference substance with Paeonol reference substance in right amount, accurately weighed, plus methyl alcohol makes every ml
In containing 20 μ g of 40 μ g of polygonin and Paeonol mixed solution, obtain final product；
The preparation precision of need testing solution measures this product 1ml, puts in 10ml measuring bottles, plus methanol dilution is to scale, shakes up, filtration,
Subsequent filtrate is taken as need testing solution；
Determination method is accurate respectively to draw reference substance and each 10 μ l of need testing solution, injects liquid chromatograph, determines, obtain final product.
2. the method for inspection of acrobatic fighting general tincture according to claim 1, it is characterised in that the acrobatic fighting general tincture is by following
Prepared by step：Take giant knotweed 150g, curcuma zedoary 100g, paniculate swallowwort 50g, Ligusticum wallichii 50g, toddalia 50g, Bi roots of grass 50g, rhizome of davallia 50g,
Frankincense 6g, pseudo-ginseng 6g, Resina Draconis 1g, mountain spicy tree root and rhizome 50g, saltcake 10g, menthol 4g totally ten three taste, except frankincense, saltcake, Resina Draconis,
Outside menthol, pseudo-ginseng is individually ground into eight tastes such as most meal, remaining giant knotweed and is also ground into most meal together, puts in container, adds
50% ethanol 1800ml, closed, impregnate 40 days；Filtration, filtrate are standby；Frankincense, saltcake, Resina Draconis are ground respectively, are added above-mentioned
In filtrate, stir evenly, closed, stand 15 days；Supernatant is taken, menthol is added, is stirred to dissolve, plus 50% ethanol to total amount is
1000ml, stirs evenly, and obtains final product.
3. the method for inspection of acrobatic fighting general tincture according to claim 2, it is characterised in that：During the most meal refers to and can pass through
The medicinal powder of a number sieve of state's pharmacopeia.
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