CN102764356A - Method for discriminating Wenweishu capsules - Google Patents

Method for discriminating Wenweishu capsules Download PDF

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Publication number
CN102764356A
CN102764356A CN2011101112015A CN201110111201A CN102764356A CN 102764356 A CN102764356 A CN 102764356A CN 2011101112015 A CN2011101112015 A CN 2011101112015A CN 201110111201 A CN201110111201 A CN 201110111201A CN 102764356 A CN102764356 A CN 102764356A
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solution
reference substance
test
wenweishu
water
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顾建光
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Abstract

The invention relates to a method for discriminating Wenweishu capsules. The method comprises steps of a Wenweishu capsule discrimination method, a Psoralea corylifolia discrimination method and the like. The discrimination method provided by the invention is simple and rapid to operate, and can be used to effectively control the quality of the product.

Description

The discrimination method of WENWEISHU JIAONANG
Technical field
The present invention relates to a kind of discrimination method of Chinese patent medicine, especially a kind of discrimination method of WENWEISHU JIAONANG.
Background technology
WENWEISHU JIAONANG is Radix Codonopsis, Radix Aconiti Lateralis Preparata (system), the Radix Astragali (processing), Cortex Cinnamomi, Rhizoma Dioscoreae, Herba Cistanches (system), the Rhizoma Atractylodis Macrocephalae (stir-fry), Fructus Crataegi (stir-fry), Fructus Mume, Pericarpium Citri Reticulatae and the capsule of Fructus Psoraleae through being processed into, strengthening the body resistance, stomach warming nourishing the stomach; Promoting the circulation of QI to relieve pain in supporing yang the warming up, are used for chronic atrophic gastritis, the caused stomach wrist of chronic gastritis cold type of pain; Abdominal distention, belch, poor appetite; Fear of cold, unable disease such as grade.Existing WENWEISHU JIAONANG discrimination method exists that precision is not high, problems such as deviation appear in repeatability greatly, easily, quality that can not the better controlled product.
Summary of the invention
The technical problem that the present invention will solve is: provide a kind of to WENWEISHU JIAONANG discrimination method fast, efficiently and easily.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of discrimination method of WENWEISHU JIAONANG, its method is:
(1), get WENWEISHU JIAONANG content 2g, porphyrize adds ethanol 70ml, puts in the water-bath warm macerating 1.5 hours; Filter, filtrating is concentrated into 15ml, filtrate for later use; Get filtrating 4ml, put evaporate to dryness in the water-bath, residue adds glacial acetic acid 2ml makes dissolving; In addition acetic anhydride and concentrated sulphuric acid volume proportion are that 20: 1 mixed liquor is a test solution number droplet, make it become two layers of liquid, and it is red to puce that liquid layer junction place shows;
(2), get above-mentioned filtrating down and drip on filter paper, add vanillin-hydrochloric acid test solution, i.e. a displaing yellow;
(3), get WENWEISHU JIAONANG content 5g, add water 35ml, supersound process 25 minutes, centrifugal, get supernatant and use the ether extraction secondary, each 20ml adds evaporate to dryness behind the ethyl acetate, residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the Hesperidin reference substance, adds methanol and processes saturated solution, as reference substance solution; According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 6 μ l of above-mentioned solution, put respectively on the silica gel g thin-layer plate for preparing with 1% sodium hydroxide solution with a slice; With ethyl acetate, first alcohol and water by volume 24: 4: 3 blended mixed liquors of proportioning be developing solvent, launch, take out; Dry, spray is put ultra-violet lamp and under 365nm, is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4), get 5 WENWEISHU JIAONANG contents, accurately claim surely, be ground into fine powder; It is fixed to get the accurate title of about 1.3g, puts in the cable type extractor according, and adding an amount of chloroform and ethanol is 7: 2 blended mixed liquors by volume; Reflux 4.5 hours, extracting solution is put evaporate to dryness in the water-bath, and residue is used anhydrous alcohol solution; Quantitatively be transferred among the 10ml and be diluted to scale, shake up, as need testing solution;
(5), get the psoralen reference substance, add dehydrated alcohol and process the solution that every 1ml contains 0.2mg, as reference substance solution; Look for thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw need testing solution and above-mentioned reference substance solution 6 μ l in (4), put respectively on a slice silica gel g thin-layer plate; With petroleum ether and ethyl acetate by volume 5: 2 blended mixed liquors of proportioning be developing solvent, launch, take out; Dry, put ultra-violet lamp and under 365nm, inspect, in the test sample chromatograph; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
The invention has the beneficial effects as follows that discrimination method of the present invention is simple to operate, fast, can effectively control the quality of product.
The specific embodiment
Below in conjunction with embodiment the present invention is done further description, yet the present invention absolutely not only is confined to described embodiment.
Concrete steps of the present invention are following:
(1), get WENWEISHU JIAONANG content 2g, porphyrize adds ethanol 70ml, puts in the water-bath warm macerating 1.5 hours; Filter, filtrating is concentrated into 15ml, filtrate for later use; Get filtrating 4ml, put evaporate to dryness in the water-bath, residue adds glacial acetic acid 2ml makes dissolving; In addition acetic anhydride and concentrated sulphuric acid volume proportion are that 20: 1 mixed liquor is a test solution number droplet, make it become two layers of liquid, and it is red to puce that liquid layer junction place shows;
(2), get above-mentioned filtrating down and drip on filter paper, add vanillin-hydrochloric acid test solution, i.e. a displaing yellow;
(3), get WENWEISHU JIAONANG content 5g, add water 35ml, supersound process 25 minutes, centrifugal, get supernatant and use the ether extraction secondary, each 20ml adds evaporate to dryness behind the ethyl acetate, residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the Hesperidin reference substance, adds methanol and processes saturated solution, as reference substance solution; According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 6 μ l of above-mentioned solution, put respectively on the silica gel g thin-layer plate for preparing with 1% sodium hydroxide solution with a slice; With ethyl acetate, first alcohol and water by volume 24: 4: 3 blended mixed liquors of proportioning be developing solvent, launch, take out; Dry, spray is put ultra-violet lamp and under 365nm, is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4), get 5 WENWEISHU JIAONANG contents, accurately claim surely, be ground into fine powder; It is fixed to get the accurate title of about 1.3g, puts in the cable type extractor according, and adding an amount of chloroform and ethanol is 7: 2 blended mixed liquors by volume; Reflux 4.5 hours, extracting solution is put evaporate to dryness in the water-bath, and residue is used anhydrous alcohol solution; Quantitatively be transferred among the 10ml and be diluted to scale, shake up, as need testing solution;
(5), get the psoralen reference substance, add dehydrated alcohol and process the solution that every 1ml contains 0.2mg, as reference substance solution; Look for thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw need testing solution and above-mentioned reference substance solution 6 μ l in (4), put respectively on a slice silica gel g thin-layer plate; With petroleum ether and ethyl acetate by volume 5: 2 blended mixed liquors of proportioning be developing solvent, launch, take out; Dry, put ultra-violet lamp and under 365nm, inspect, in the test sample chromatograph; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and through above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the description, must confirm its technical scope according to the claim scope.

Claims (1)

1. the discrimination method of a WENWEISHU JIAONANG, its method is:
(1), get WENWEISHU JIAONANG content 2g, porphyrize adds ethanol 70ml, puts in the water-bath warm macerating 1.5 hours; Filter, filtrating is concentrated into 15ml, filtrate for later use; Get filtrating 4ml, put evaporate to dryness in the water-bath, residue adds glacial acetic acid 2ml makes dissolving; In addition acetic anhydride and concentrated sulphuric acid volume proportion are that 20: 1 mixed liquor is a test solution number droplet, make it become two layers of liquid, and it is red to puce that liquid layer junction place shows;
(2), get above-mentioned filtrating down and drip on filter paper, add vanillin-hydrochloric acid test solution, i.e. a displaing yellow;
(3), get WENWEISHU JIAONANG content 5g, add water 35ml, supersound process 25 minutes, centrifugal, get supernatant and use the ether extraction secondary, each 20ml adds evaporate to dryness behind the ethyl acetate, residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the Hesperidin reference substance, adds methanol and processes saturated solution, as reference substance solution; According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 6 μ l of above-mentioned solution, put respectively on the silica gel g thin-layer plate for preparing with 1% sodium hydroxide solution with a slice; With ethyl acetate, first alcohol and water by volume 24: 4: 3 blended mixed liquors of proportioning be developing solvent, launch, take out; Dry, spray is put ultra-violet lamp and under 365nm, is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4), get 5 WENWEISHU JIAONANG contents, accurately claim surely, be ground into fine powder; It is fixed to get the accurate title of about 1.3g, puts in the cable type extractor according, and adding an amount of chloroform and ethanol is 7: 2 blended mixed liquors by volume; Reflux 4.5 hours, extracting solution is put evaporate to dryness in the water-bath, and residue is used anhydrous alcohol solution; Quantitatively be transferred among the 10ml and be diluted to scale, shake up, as need testing solution;
(5), get the psoralen reference substance, add dehydrated alcohol and process the solution that every 1ml contains 0.2mg, as reference substance solution; Look for thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw need testing solution and above-mentioned reference substance solution 6 μ l in (4), put respectively on a slice silica gel g thin-layer plate; With petroleum ether and ethyl acetate by volume 5: 2 blended mixed liquors of proportioning be developing solvent, launch, take out; Dry, put ultra-violet lamp and under 365nm, inspect, in the test sample chromatograph; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
CN2011101112015A 2011-04-30 2011-04-30 Method for discriminating Wenweishu capsules Pending CN102764356A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103405618A (en) * 2013-08-09 2013-11-27 陕西步长高新制药有限公司 TCM (Traditional Chinese Medicine) composition for invigorating kidney and strengthening Yang and preparation and detection methods of TCM composition
CN103405616A (en) * 2013-08-09 2013-11-27 陕西步长高新制药有限公司 TCM (Traditional Chinese Medicine) composition for invigorating kidney and strengthening Yang and preparation and detection methods of TCM composition
CN105929101A (en) * 2016-04-20 2016-09-07 广西壮族自治区梧州食品药品检验所 Method for qualitative identification of hesperidin in throat-clearing granule by using macroporous resin adsorption process

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103405618A (en) * 2013-08-09 2013-11-27 陕西步长高新制药有限公司 TCM (Traditional Chinese Medicine) composition for invigorating kidney and strengthening Yang and preparation and detection methods of TCM composition
CN103405616A (en) * 2013-08-09 2013-11-27 陕西步长高新制药有限公司 TCM (Traditional Chinese Medicine) composition for invigorating kidney and strengthening Yang and preparation and detection methods of TCM composition
CN103405616B (en) * 2013-08-09 2015-06-10 陕西步长高新制药有限公司 TCM (Traditional Chinese Medicine) composition for invigorating kidney and strengthening Yang and preparation and detection methods of TCM composition
CN105929101A (en) * 2016-04-20 2016-09-07 广西壮族自治区梧州食品药品检验所 Method for qualitative identification of hesperidin in throat-clearing granule by using macroporous resin adsorption process

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Application publication date: 20121107