CN102078386A - Method for detecting Xiaoyao mixture - Google Patents
Method for detecting Xiaoyao mixture Download PDFInfo
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- CN102078386A CN102078386A CN200910186585XA CN200910186585A CN102078386A CN 102078386 A CN102078386 A CN 102078386A CN 200910186585X A CN200910186585X A CN 200910186585XA CN 200910186585 A CN200910186585 A CN 200910186585A CN 102078386 A CN102078386 A CN 102078386A
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Abstract
The invention relates to a method for detecting a Xiaoyao mixture. The method for detecting the Xiaoyao mixture comprises the steps of discriminating and determining the content, wherein thin layer chromatography is adopted in the discriminating step, and liquorice is taken as a control medicinal material to discriminate liquorice in the Xiaoyao mixture; and high efficiency liquid chromatography is adopted to determine the content of paeoniflorin in the Xiaoyao mixture in the content determining step.
Description
Technical field
The present invention relates to a kind of detection method of Chinese medicine preparation, specifically, the present invention relates to the detection method of the carefree mixture of Chinese patent medicine.
Background technology
Carefree mixture is a kind of soothing liver and strengthening spleen, and the Chinese patent medicine of nourishing blood for regulating menstruation has gone on the market for many years in China, the clinical depression of liver-QI that is used for, and distending pain in the chest and hypochondrium is had a dizzy spell, and loss of appetite, curative effects such as menoxenia are certainly.Carefree mixture is prepared from by the common process of Chinese patent medicine mixture by Chinese crude drug Radix Bupleuri, Radix Angelicae Sinensis, the Radix Paeoniae Alba, the Rhizoma Atractylodis Macrocephalae, Poria, Radix Glycyrrhizae (processed with honey), Herba Menthae.The quality standard of this product records in the 11 in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, and standard is numbered WS3-B-2221-96.Only there is the qualitative chemical reaction of Radix Bupleuri to differentiate that its specificity is relatively poor, and without any quantitative detection method, is unfavorable for controlling the product quality of carefree mixture in this standard.
The objective of the invention is strong for the qualitative identification method that overcomes only a kind of medical material in the present carefree mixture quality standard, specificity, as to be unfavorable for controlling product quality shortcoming.Provide a kind of specificity strong, and more can accurately control the method for quality control of the carefree mixture of product quality.
Summary of the invention
Carefree mixture detection method of the present invention comprises and differentiating and the step of assay:
Thin layer chromatography is adopted in described discriminating, with the Radix Glycyrrhizae control medicinal material, differentiates the Radix Glycyrrhizae in the carefree mixture;
Described assay adopts content of paeoniflorin in the carefree mixture of high effective liquid chromatography for measuring.
Discrimination method of the present invention, preferably: get carefree mixture 30ml, with water saturated n-butanol extraction 2 times, each 20ml, merge n-butyl alcohol liquid, use the saturated water washing of n-butyl alcohol 2 times, each 10ml, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1g in addition, it is an amount of to add water, decocts 30 minutes, takes out, put cold, filtration, filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution and Radix Glycyrrhizae control medicinal material solution respectively, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, put under the ultra-violet lamp (365nm) and inspect, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Content assaying method of the present invention, preferably:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.1% phosphoric acid (15: 85) is mobile phase; Detect wavelength 230nm.Number of theoretical plate calculates by the peoniflorin peak should be not less than 2000.
It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds Diluted Alcohol and makes the solution that every 1ml contains 50ug, promptly.
The preparation precision of need testing solution is measured this product 3ml, puts in the 25ml measuring bottle, adds Diluted Alcohol alcohol and is diluted to scale, shakes up, and filters, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every 1ml of this product contains the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, must not be less than 2.6mg.
Content assaying method of the present invention is through the methodology checking, and negative sample is noiseless to measuring, and peoniflorin presents good linear relationship in the 0.00-0.10mg/ml scope, and the linear correlation degree is 0.9920.This extracting method method response rate is 98.3% (n=5), RSD=1.7%.Measure ten batches of carefree mixture samples with this method, content of paeoniflorin result is as follows:
The detection method of carefree mixture of the present invention has not only increased the qualitative identification method but also has increased the Content Measurement of Effective Ingredient in Happiness method, has improved the specificity and the quality stability of carefree mixture method of quality control, has guaranteed the safety and the effectiveness of people's medications.The method of quality control of carefree mixture of the present invention both can be used for controlling the quality of carefree mixture, can be used for controlling the quality of other dosage form of identical prescription such as granule etc. again.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Get carefree mixture.
This product 5ml is got in [discriminating] (1), and evaporate to dryness, residue add ethanol 5ml makes dissolving, filters, and gets filtrate 0.5ml, adds methanol solution (1 → 30) 0.5ml and the phosphatase 11 ml of paradime thylaminobenzaldehyde, and mixing is put in the water-bath and heated, and fades in redness.
(2) get carefree mixture 30ml, with water saturated n-butanol extraction 2 times, each 20ml merges n-butyl alcohol liquid, with the saturated water washing of n-butyl alcohol 2 times, and each 10ml, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1g in addition, it is an amount of to add water, decocts 30 minutes, takes out, put cold, filtration, filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution and Radix Glycyrrhizae control medicinal material solution respectively, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, put under the ultra-violet lamp (365nm) and inspect, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
[inspection] should meet every regulation relevant under the mixture item (appendix IJ of Chinese Pharmacopoeia version in 2005).
[assay] takes high picture liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D) mensuration.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.1% phosphoric acid (15: 85) is mobile phase; Detect wavelength 230nm.Number of theoretical plate calculates by the peoniflorin peak should be not less than 2000.
It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds Diluted Alcohol and makes the solution that every 1ml contains 50ug, promptly.
The preparation precision of need testing solution is measured this product 3ml, puts in the 25ml measuring bottle, adds Diluted Alcohol alcohol and is diluted to scale, shakes up, and filters, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every 1ml of this product contains the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, be 2.74mg.
Claims (6)
1. the detection method of a carefree mixture is characterized in that, comprises the step of discriminating and assay.
2. the detection method of claim 1 is characterized in that, thin layer chromatography is adopted in described discriminating, with the Radix Glycyrrhizae control medicinal material, differentiates the Radix Glycyrrhizae in the carefree mixture.
3. the detection method of claim 1 is characterized in that, described assay adopts content of paeoniflorin in the carefree mixture of high effective liquid chromatography for measuring.
4. the detection method of claim 1, discrimination method wherein, step is as follows: get carefree mixture 30ml, with water saturated n-butanol extraction 2 times, each 20ml merges n-butyl alcohol liquid, with the saturated water washing of n-butyl alcohol 2 times, each 10ml, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution, extracting liquorice control medicinal material 1g in addition, it is an amount of to add water, decocted 30 minutes, take out, put coldly, filter, filtrate is concentrated into 20ml, shine medical material solution in pairs with legal system,, draw need testing solution and Radix Glycyrrhizae control medicinal material solution respectively according to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with ethyl acetate-formic acid-glacial acetic acid-water=15: 1: 1: 2 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, puts under the 365nm ultra-violet lamp and inspects, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
5. the detection method of claim 1, content assaying method wherein, step is as follows:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.1% phosphoric acid=15: 85 is mobile phase; Detect wavelength 230nm, number of theoretical plate calculates by the peoniflorin peak should be not less than 2000,
It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and add Diluted Alcohol and make the solution that every 1ml contains 50ug, that is,
The preparation precision of need testing solution is measured this product 3ml, puts in the 25ml measuring bottle, adds Diluted Alcohol alcohol and is diluted to scale, shakes up, filter, that is,
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, that is,
The every 1ml of this product contains the Radix Paeoniae Alba in peoniflorin, must not be less than 2.6mg.
6. the detection method of claim 1, step is as follows:
This product 5ml is got in [discriminating] (1), and evaporate to dryness, residue add ethanol 5ml makes dissolving, filters, and gets filtrate 0.5ml, adds methanol solution (1 → 30) 0.5ml and the phosphatase 11 ml of paradime thylaminobenzaldehyde, and mixing is put in the water-bath and heated, and fades in redness,
(2) get carefree mixture 30ml, with water saturated n-butanol extraction 2 times, each 20ml, merge n-butyl alcohol liquid, use the saturated water washing of n-butyl alcohol 2 times, each 10ml, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, and as need testing solution, other is extracting liquorice control medicinal material 1g, it is an amount of to add water, decocted 30 minutes, and took out, put cold, filter, filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system, according to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution and Radix Glycyrrhizae control medicinal material solution respectively, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with ethyl acetate-formic acid-glacial acetic acid-water=15: 1: 1: 2 be developing solvent, expansion, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃, put under the 365nm ultra-violet lamp and inspect, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color
[inspection] should meet relevant every regulation under an appendix IJ of Chinese Pharmacopoeia version in 2005 the mixture item,
[assay] takes the high picture liquid chromatography for measuring of Chinese Pharmacopoeia version in 2005 appendix VI D,
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.1% phosphoric acid=15: 85 is mobile phase; Detect wavelength 230nm, number of theoretical plate calculates by the peoniflorin peak should be not less than 2000,
It is an amount of that the peoniflorin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and add Diluted Alcohol and make the solution that every 1ml contains 50ug, that is,
The preparation precision of need testing solution is measured this product 3ml, puts in the 25ml measuring bottle, adds Diluted Alcohol alcohol and is diluted to scale, shakes up, filter, that is,
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, that is,
The every 1ml of this product contains the Radix Paeoniae Alba in peoniflorin, is 2.74mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910186585XA CN102078386A (en) | 2009-11-30 | 2009-11-30 | Method for detecting Xiaoyao mixture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910186585XA CN102078386A (en) | 2009-11-30 | 2009-11-30 | Method for detecting Xiaoyao mixture |
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| Publication Number | Publication Date |
|---|---|
| CN102078386A true CN102078386A (en) | 2011-06-01 |
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ID=44084711
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|---|---|---|---|
| CN200910186585XA Pending CN102078386A (en) | 2009-11-30 | 2009-11-30 | Method for detecting Xiaoyao mixture |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105116066A (en) * | 2015-07-28 | 2015-12-02 | 渠县金穗农业科技有限公司 | Method for detecting paeoniflorin content of white peony root-red date-lemon functional beverage |
| CN106841501A (en) * | 2017-03-08 | 2017-06-13 | 北京市药品检验所 | Simple and fast differentiates the thin-layered chromatography of Radix Glycyrrhizae, swollen fruit Radix and glycyrrhiza glabra |
-
2009
- 2009-11-30 CN CN200910186585XA patent/CN102078386A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105116066A (en) * | 2015-07-28 | 2015-12-02 | 渠县金穗农业科技有限公司 | Method for detecting paeoniflorin content of white peony root-red date-lemon functional beverage |
| CN106841501A (en) * | 2017-03-08 | 2017-06-13 | 北京市药品检验所 | Simple and fast differentiates the thin-layered chromatography of Radix Glycyrrhizae, swollen fruit Radix and glycyrrhiza glabra |
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Application publication date: 20110601 |