CN102068656B - Quality control method for traditional Chinese medicinal preparation epilepsy pills - Google Patents
Quality control method for traditional Chinese medicinal preparation epilepsy pills Download PDFInfo
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- CN102068656B CN102068656B CN200910228362A CN200910228362A CN102068656B CN 102068656 B CN102068656 B CN 102068656B CN 200910228362 A CN200910228362 A CN 200910228362A CN 200910228362 A CN200910228362 A CN 200910228362A CN 102068656 B CN102068656 B CN 102068656B
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Abstract
The invention belongs to the technical field of traditional Chinese medicine and relates to a quality control method for traditional Chinese medicinal preparation epilepsy pills which are prepared from traditional Chinese medicinal materials. In a quality standard, megnolia hypoleuca and Yanhusuo (a traditional Chinese medicine which is mainly produced in Zhejiang, China) are set as reference products to identify whether an epilepsy pill prescription contains megnolia hypoleuca and Yanhusuo components or not by thin layer chromatography; and the content of magnolol in the medicament is tested by efficient liquid phase chromatography. A quantitative index that the content of magnolol cannot be less than 1.04mg in each gram of magnolol and an inspection method for the quantitative index make the quality standard more perfect, so the quality of the medicament can be controlled strictly and the product quality can be ensured to be improved; and the revised quality standard enhances the quality control on the medicament.
Description
Technical field
The invention belongs to the technical field of Chinese patent drug, relating to the Chinese crude drug is the detection method of the insane ball of a kind of Chinese medicine preparation epilepsy processed of raw material.
Background technology
The insane ball of epilepsy is a kind of classical Chinese patent drug, the standard WS of the Ministry of Public Health
3-B-1741-94 record prescription and quality standard:
Prescription: the prepared RHIZOMA PINELLIZE without adju-vant 60g bark of official magnolia (ginger system) 60g Tabasheer 60g
Notopterygium root 60g root tuber of aromatic turmeric 60g tangerine 60g
Rhizoma arisaematis (system) 60g rhizoma Gastrodiae 36g rhizoma cyperi (vinegar system) 36g
Corydalis tuber (vinegar system) 36g root of Chinese wild ginger 36g Fructus Aurantii (bran stir-fry) 36g
Triangular (vinegar system) 36g rascal (vinegar system) 36g dalbergia wood 36g
Mustard seed (stir-fry) 24g agalloch eaglewood 24g curcuma zedoary (vinegar system) 24g
The windproof 24g antelope's horn of root of three-nerved spicebush 24g 12.55g
Method for making: above 20 simply, and the antelope's horn file is ground into impalpable powder, and 20 flavors such as prepared RHIZOMA PINELLIZE without adju-vant are ground into fine powder, with above-mentioned antelope's horn powder facing-up, sieve mixing, water pill, drying.The dried ball of every 500g, in addition with forging Lapis Micae Aureus powder 60g dressing, polishing, drying promptly gets.
Inspection: should meet each item regulation (8 pages of appendix) relevant under the pill item.
At present the document about the method for quality control of magnolol and honokiol, corydalis tuber has a lot, but Shang Weijian and the above-mentioned disclosed standard WS of the Ministry of Public Health
3The insane ball prescription of-B-1741-94 epilepsy is similar or identical; Proportioning is different; The improved document of the product standard that effect is similar; But also there are shortcomings such as discriminating project, discriminating means, content assaying method imperfection in the standard of prior art,, need improve target level of product quality for improving the product quality of Chinese medicine.
Summary of the invention
The objective of the invention is to overcome the insane ball standard of the epilepsy weak point of prior art, a kind of detection method of the insane ball of epilepsy that can the qualitative and quantitative analysis drug ingedient is provided.
In order to reach the technical scheme that the object of the invention adopts be: the detection method of the insane ball of a kind of Chinese medicine preparation epilepsy, wherein said pharmaceutical formulation are by Chinese crude drug:
The prepared RHIZOMA PINELLIZE without adju-vant 60g bark of official magnolia (ginger system) 60g Tabasheer 60g
The tangerine 60g of notopterygium root 60g root tuber of aromatic turmeric 60g
Rhizoma arisaematis (system) 60g rhizoma Gastrodiae 36g rhizoma cyperi (vinegar system) 36g
Corydalis tuber (vinegar system) 36g root of Chinese wild ginger 36g Fructus Aurantii (bran stir-fry) 36g
Triangular (vinegar system) 36g rascal (vinegar system) 36g dalbergia wood 36g
Mustard seed (stir-fry) 24g agalloch eaglewood 24g curcuma zedoary (vinegar system) 24g
The windproof 24g antelope's horn of root of three-nerved spicebush 24g 12.55g forms, and method for making: above 20 simply, and the antelope's horn file is ground into impalpable powder; 20 flavors such as prepared RHIZOMA PINELLIZE without adju-vant are ground into fine powder, with above-mentioned antelope's horn powder facing-up, sieve; Mixing, water pill, drying; The dried ball of every 500g, in addition with forging Lapis Micae Aureus powder 60g dressing, polishing, drying promptly gets, and it is characterized in that: the step of its method is:
(1) be control medicinal material with the bark of official magnolia, corydalis tuber, thin-layered chromatography differentiates in the insane ball prescription of epilepsy whether contain the bark of official magnolia, corydalis tuber composition;
(2) with the magnolol be reference substance, high performance liquid chromatography detects the content of magnolol in the insane ball prescription of epilepsy.
The detection method of the insane ball of described Chinese medicine preparation epilepsy is characterized in that: described thin-layered chromatography differentiates that the method that whether contains bark of official magnolia composition in the insane ball prescription of epilepsy is: get these article 3g, grind; Add methyl alcohol 20ml; Sonicated 30 minutes filters, the filtrating evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets bark of official magnolia control medicinal material 0.5g and shines medicinal material solution in pairs with legal system; According to the thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-methyl alcohol; Benzene: methyl alcohol=27: 1, launch, take out; Dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
Described thin-layered chromatography differentiates that the method that whether contains the corydalis tuber composition in the insane ball prescription of epilepsy is: get these article powder 3g, add methyl alcohol 50ml, sonicated 30 minutes filters; The filtrating evaporate to dryness, residue adds water 10ml makes dissolving, adds strong ammonia solution and transfers to alkalescence; With extracted by ether 3 times, each 10ml merges ether solution; Volatilize, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets corydalis tuber control medicinal material 0.5g, shines medicinal material solution in pairs with legal system; According to the thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on the same silica gel g thin-layer plate of processing with 1% sodium hydroxide solution; With toluene-acetone is developping agent, toluene: acetone=9: 2, launch; Take out, dry, put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color
The detection method of the insane ball of described Chinese medicine preparation epilepsy is characterized in that: be reference substance with the magnolol, the method that liquid phase chromatography detects the content of magnolol in the insane ball prescription of epilepsy is:
(1) chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol: water: glacial acetic acid=78: 22: 0.5 is a moving phase; The detection wavelength is 294nm; Number of theoretical plate calculates by the magnolol peak should be not less than 2000, and the degree of separation of magnolol peak and adjacent peak is answered requirement up to specification;
(2) preparation of reference substance solution: it is an amount of to get the magnolol reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 40 μ g, promptly gets;
(3) preparation of need testing solution: sample thief 3g, porphyrize is got powder 1.0g, and accurate the title, decide, and puts in the tool plug conical flask; Precision is measured methyl alcohol 25ml, claims decide weight, and reflux 40 minutes is put coldly, and weight decided in title; Supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, promptly get;
(4) determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get; The every gram of these article contains magnolol must not be less than 1.04mg.
The invention beneficial effect: what be provided with in the quality standard is control medicinal material with the bark of official magnolia, corydalis tuber, and thin-layered chromatography differentiates in the insane ball prescription of epilepsy whether contain the bark of official magnolia, the corydalis tuber composition is differentiated project; Content with magnolol in this medicine of high effective liquid chromatography for measuring; Supply the every gram of test agent to contain the quantitative target and the method for inspection that magnolol must not be less than 1.04mg, make quality standard comparatively perfect, revised quality standard, the quality control that has improved medicine.
Description of drawings
Fig. 1 bark of official magnolia thin layer is differentiated spectrogram.
Fig. 2 corydalis tuber thin layer is differentiated spectrogram.
The HPLC collection of illustrative plates of Fig. 3 magnolol reference substance.
The HPLC collection of illustrative plates of Fig. 4 test sample.
The HPLC collection of illustrative plates of Fig. 5 blank article.
Fig. 6 linear diagram.
Embodiment
Below in conjunction with embodiment, the present invention is further specified the insane ball quality standard of epilepsy after embodiment 1 improves:
Prescription: the prepared RHIZOMA PINELLIZE without adju-vant 60g bark of official magnolia (ginger system) 60g Tabasheer 60g
The tangerine 60g of notopterygium root 60g root tuber of aromatic turmeric 60g
Rhizoma arisaematis (system) 60g rhizoma Gastrodiae 36g rhizoma cyperi (vinegar system) 36g
Corydalis tuber (vinegar system) 36g root of Chinese wild ginger 36g Fructus Aurantii (bran stir-fry) 36g
Triangular (vinegar system) 36g rascal (vinegar system) 36g dalbergia wood 36g
Mustard seed (stir-fry) 24g agalloch eaglewood 24g curcuma zedoary (vinegar system) 24g
The windproof 24g antelope's horn of root of three-nerved spicebush 24g 12.55g
Method for making: above 20 simply, and the antelope's horn file is ground into impalpable powder, and 20 flavors such as prepared RHIZOMA PINELLIZE without adju-vant are ground into fine powder, with above-mentioned antelope's horn powder facing-up, sieve mixing, water pill, drying.The dried ball of every 500g, in addition with forging Lapis Micae Aureus powder 60g dressing, polishing, drying promptly gets.
Proterties: these article are pale brown look to the filemot water-bindered pill, show pale brown look after removing coat; Distinguish the flavor of sweet, little hardship, suffering.
Inspection: should meet each item regulation (8 pages of appendix) relevant under the pill item.
Differentiate: (1) bark of official magnolia is differentiated: get these article 3g, grind, add methyl alcohol 20ml, ultrasonic place 30 minutes filters, the filtrating evaporate to dryness, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets bark of official magnolia control medicinal material 0.5g and shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With benzene-methyl alcohol=27: 1 was developping agent, launched, and took out; Dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(2) corydalis tuber is differentiated: get these article powder 3g, add methyl alcohol 50ml, ultrasonic place 30 minutes filters, the filtrating evaporate to dryness; Residue adds water 10ml makes dissolving, and add strong ammonia solution and transfer to alkalescence, with extracted by ether 3 times, each 10ml; Merge ether solution, volatilize, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets corydalis tuber control medicinal material 0.5g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005); Drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on the same silica gel g thin-layer plate of processing with 1% sodium hydroxide solution, is developping agent with toluene-acetone=9: 2; Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.Assay: the photograph high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 D) measure.
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methanol-water-glacial acetic acid=78: 22: 0.5 is a moving phase; The detection wavelength is 294nm.Number of theoretical plate calculates by the magnolol peak should be not less than 2000, and the degree of separation of magnolol peak and adjacent peak should requirement up to specification.
It is an amount of that the magnolol reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 40 μ g, promptly gets.
The preparation sample thief 3g of need testing solution, porphyrize is got powder 1.0g, and accurate the title, decide, and puts in the tool plug conical flask; Precision is measured methyl alcohol 25ml, claims decide weight, and reflux 40 minutes is put coldly, and weight decided in title; Supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, promptly get.
Accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get.The every gram of these article contains magnolol must not be less than 1.04mg.
Function with cure mainly: flat liver is had a respite, and falls phlegm and treats epilepsy.Be used for closing in the phlegm heat, faint suddenly, slobbering, brothers twitch.
Usage and consumption: oral, the 3g that is grown up a time, 1g of four to ten years old children's, 1.5g of ten years old to 15 years old children, 2 times on the one.Attention: the pregnant woman follows the doctor's advice and takes.Specification: every bottled 3g; Storage: airtight, protection against the tide.
The insane ball quality standard of embodiment 2 epilepsies is drafted explanation: no thin layer is differentiated and assay in the insane ball proper mass of the epilepsy standard, and the thin layer that increases the bark of official magnolia, corydalis tuber is differentiated the assay of magnolol in the magnolia obovata.
One. thin layer is differentiated
1. the discriminating of the bark of official magnolia
1.1 material and reagent: methyl alcohol, benzene: analyze pure
Bark of official magnolia control medicinal material: Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 121285-200301
1.2 the preparation of need testing solution: get these article powder 3g, add methyl alcohol 20ml, sonicated 30 minutes leaves standstill, filters, and the filtrating evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.
1.3 the preparation of control medicinal material solution: get bark of official magnolia control medicinal material 0.5g, shine medicinal material solution in pairs with legal system.
1.4 the preparation of blank article solution: by prescription, technology, except that the bark of official magnolia, prepare the blank article, again the blank article are ground into fine powder, prepare blank article solution according to the need testing solution preparation method.
1.5 experimental technique: according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test; Drawing above-mentioned 3 kinds of solution points respectively on same block of silica G plate, is developping agent with benzene-methyl alcohol=27: 1, launches; Take out; Dry, spray is with 5% vanillic aldehyde sulfuric acid chromogenic reagent, and it is clear under 105 ℃, to be heated to spot colour developing.The test sample chromatogram with control medicinal material chromatogram relevant position on show the spot of same color, the blank article are noiseless.The result sees Fig. 1.Among Fig. 11 is that reference substance 2 is the blank article for test sample 3
2. the discriminating of corydalis tuber
2.1 material and reagent: methyl alcohol, ether, toluene, acetone: analyze pure
Corydalis tuber control medicinal material: Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 120928-200403
2.2 the preparation of need testing solution: get these article powder 3g, add methyl alcohol 50ml, sonicated 30 minutes filters; The filtrating evaporate to dryness, residue adds water 10ml makes dissolving, adds strong ammonia solution and transfers to alkalescence; With extracted by ether 3 times, each 10ml merges ether solution; Volatilize, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.
2.3 the preparation of control medicinal material solution: other gets corydalis tuber control medicinal material 0.5g, shines medicinal material solution in pairs with legal system.
2.4 the preparation of blank article solution: by prescription, technology, except that corydalis tuber, prepare the blank article, again the blank article are ground into fine powder, prepare blank article solution according to the need testing solution preparation method.
2.5 experimental technique: according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test; Drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on the same silica gel g thin-layer plate of processing with 1% sodium hydroxide solution, is developping agent with toluene-acetone=9: 2; Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.Blank article chromatogram is noiseless.The result sees Fig. 2.Among Fig. 21 is that reference substance 2 is the blank article for test sample 3.
Two. the assay of magnolol
2.1 instrument and material
Instrument: Waters 2695 high performance liquid chromatographs, Waters 2487 detecting devices; Sartorius CP224S. electronic balance.
Material: magnolol reference substance: check institute available from Chinese pharmaceutical biological product; Lot number: 110713-200208
Glacial acetic acid: analyze pure
Methyl alcohol is chromatographically pure
Deionized water
2.2 experimental technique: with reference to " method under 2005 editions one magnolia medicament assay item of Chinese pharmacopoeia, but because the honokiol peak has assorted peak to disturb, so only formulate the magnolol content measuring standard.
2.2.1 chromatographic condition: select C for use
18Chromatographic column, column temperature are 30 ℃, and " the detection wavelength under 2005 editions one magnolia medicament assay item of Chinese pharmacopoeia is 294nm, and flow velocity is 0.8ml/min to detect wavelength reference.
2.2.2 the selection of moving phase: with reference to " 2005 editions one magnolia medicament assay item of Chinese pharmacopoeia current downflow phase; (1) methanol-water (78: 22) on probation, (2) methanol-water-glacial acetic acid (78: 22: 0.5) etc. are as moving phase; The result separates best in magnolol peak when adopting (2); And retention time is suitable, so choosing (2) is as moving phase.
2.2.3 the preparation of reference substance solution: it is an amount of to get the magnolol reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 40 μ g, as reference substance solution.See Fig. 3
2.2.4 need testing solution preparation
2.2.4.1 the selection of method for distilling: the result shows employing method 2 preparation samples, and magnolol content is higher, extracts fully.
The selection of table 1 method for distilling
2.2.4.2 the selection of extraction time: choose difference extraction time sample introduction, the result sees table 2, and the result shows employing method 3 preparation samples, and magnolol content is higher, extracts fully.
The selection of table 2 extraction time
2.2.4.3 confirm the preparation method of need testing solution: sample thief 3g, porphyrize is got powder 1.0g, and accurate the title, decide; Put in the tool plug conical flask, precision is measured methyl alcohol 25ml, claims to decide weight, reflux 40 minutes; Put coldly, claim to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol; Filter, get subsequent filtrate, promptly get.See Fig. 4
2.2.4.4 blank article formulations prepared from solutions: by prescription, technology, remove the bark of official magnolia and prepare the blank article, again the blank article are ground into fine powder, prepare blank article solution by the need testing solution preparation method.See Fig. 5
2.3 methodological study
2.3.1 linear relationship: get magnolol reference substance solution (concentration: 0.02952mg/ml) difference sample introduction 2 μ l, 4 μ l, 8 μ l, 12 μ l; 16 μ l, 20 μ l, 24 μ l; 30 μ l inject high performance liquid chromatograph, are horizontal ordinate with the sampling volume, are that ordinate is done linear regression with the peak area.The result sees table 3.Linearity curve is as shown in Figure 6.Fig. 6 gets magnolol reference substance solution sample introduction linearity curve respectively, gets regression equation by data and is: y=A+Bx=60272.68x-12226.67, r=0.9999957 result show that magnolol is good in 0.05904～0.8856 μ g scope internal linear relation.
2.3.2 precision experiment: to same need testing solution continuous sample introduction 6 times, measure relative standard deviation RSD=0.2%, show that precision is good.The result sees table 5
The linear result that investigates of table 3
The experiment of table 5 precision
2.3.3 reappearance experiment: get 6 parts of same lot sample article; According to preparation method's preparation of need testing solution, each duplicate samples solution sample introduction is got the mean value of its peak area for twice, and the RSD that measures magnolol content is 1.70%; The result shows that reappearance is good, and the result sees table 6.
The experiment of table 6 reappearance
2.3.4 stability experiment: same need testing solution is every at a distance from 2 hours sample introductions once, and continuous sample introduction 6 times carries out assay respectively, and the RSD value is 0.77%, and the result is presented at that need testing solution has good stability in 10 hours, and the result sees like table 7.
Table 7 stability experiment
2.3.5 recovery experiment: get 6 parts in the insane ball of epilepsy (known content 1.286mg/g) sample; Every part of 0.5g; Precision takes by weighing, and adds magnolol reference substance 0.64mg (getting concentration is the magnolol reference substance solution of 0.32mg/ml, and precision is measured 2ml and added in the test sample); Press need testing solution preparation method preparation, inject high performance liquid chromatograph and measure.Measuring the result with 6 estimates.Average recovery rate is 98.5%, RSD value=2.58%, and the show sample recovery is good as a result, and the result sees table 8.
2.3.6 sample size is measured: get three lot sample article, prepare according to the need testing solution preparation method respectively, measure three lot sample article content, the result sees table 9.
The experiment of table 8 recovery
Table 9 three lot sample article assay results
1.296 * 80%=1.04mg/g according to above three batches testing result, confirms that the content standard of magnolol must not be in the insane ball of epilepsy and is lower than 1.04mg/g.
Claims (1)
1. the method for quality control of the insane ball of Chinese medicine preparation epilepsy, wherein said pharmaceutical formulation are by Chinese crude drug:
(1) be control medicinal material with the bark of official magnolia, corydalis tuber, thin-layered chromatography differentiates in the insane ball prescription of epilepsy whether contain the bark of official magnolia, corydalis tuber composition; Thin-layered chromatography differentiates that the method that whether contains bark of official magnolia composition in the insane ball prescription of epilepsy is: get these article 3g, grind, add methyl alcohol 20ml, sonicated 30 minutes filters, the filtrating evaporate to dryness, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets bark of official magnolia control medicinal material 0.5g and shines medicinal material solution in pairs with legal system; According to the thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developping agent with benzene-methyl alcohol; Benzene: methyl alcohol=27: 1, launch, take out; Dry, spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear to be heated to spot colour developing at 105 ℃; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
Thin-layered chromatography differentiates that the method that whether contains the corydalis tuber composition in the insane ball prescription of epilepsy is: get these article powder 3g, add methyl alcohol 50ml, sonicated 30 minutes filters; The filtrating evaporate to dryness, residue adds water 10ml makes dissolving, adds strong ammonia solution and transfers to alkalescence; With extracted by ether 3 times, each 10ml merges ether solution; Volatilize, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets corydalis tuber control medicinal material 0.5g, shines medicinal material solution in pairs with legal system; According to the thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on the same silica gel g thin-layer plate of processing with 1% sodium hydroxide solution; With toluene-acetone is developping agent, toluene: acetone=9: 2, launch; Take out, dry, put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(2) with the magnolol be reference substance, the method that high performance liquid chromatography detects the content of magnolol in the insane ball prescription of epilepsy is:
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol: water: glacial acetic acid=78: 22: 0.5 is a moving phase; The detection wavelength is 294nm; Number of theoretical plate calculates by the magnolol peak should be not less than 2000, and the degree of separation of magnolol peak and adjacent peak is answered requirement up to specification;
The preparation of reference substance solution: it is an amount of to get the magnolol reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 40 μ g, promptly gets;
The preparation of need testing solution: sample thief 3g, porphyrize is got powder 1.0g, and accurate the title, decide, and puts in the tool plug conical flask; Precision is measured methyl alcohol 25ml, claims decide weight, and reflux 40 minutes is put coldly, and weight decided in title; Supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, promptly get;
Determination method: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
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| CN102309471A (en) * | 2010-06-30 | 2012-01-11 | 复旦大学 | Application of magnolol or derivative thereof to preparation of antiepileptic medicaments |
| CN102406844B (en) * | 2011-07-11 | 2014-02-12 | 李保明 | Traditional Chinese medicine preparation for treating epilepsy and its preparation method |
| CN103033585A (en) * | 2011-09-30 | 2013-04-10 | 西安千禾药业有限责任公司 | Method for detecting medicaments for treating mammitis and hyperplasia of mammary glands |
| CN104998205A (en) * | 2015-07-31 | 2015-10-28 | 周振平 | Traditional Chinese medicine for treating falling sickness mental disturbance |
| CN105213988A (en) * | 2015-10-30 | 2016-01-06 | 王玉龙 | A kind of Chinese medicine composition being used for the treatment of epilepsy and preparation method thereof |
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| Title |
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| 中华人民共和国***药典委员会.羊痫疯癫丸.《中华人民共和国***药品标准中药成方制剂第九册》.1994,78. * |
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