CN103364520A - Quality determination method of gingko honey ring compound preparation - Google Patents
Quality determination method of gingko honey ring compound preparation Download PDFInfo
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- CN103364520A CN103364520A CN2012100967063A CN201210096706A CN103364520A CN 103364520 A CN103364520 A CN 103364520A CN 2012100967063 A CN2012100967063 A CN 2012100967063A CN 201210096706 A CN201210096706 A CN 201210096706A CN 103364520 A CN103364520 A CN 103364520A
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Abstract
The invention discloses a quality determination method of a gingko honey ring compound preparation. A thin layer chromatography process is adopted to determine whether the gingko honey ring compound preparation has honey fungus powder; a high performance liquid chromatography process is adopted to test the content of adenosine in the gingko honey ring preparation. According to the quality determination method, the defect of the prior art is overcome, qualitative and quantitative determination with specificity is performed on honey fungus components in the gingko honey ring compound preparation so as to effectively reflect whether the compound preparation has the honey fungus and the content of the honey fungus in the compound preparation. According to current standards, the specificity and the reliability of the quality determination method of the gingko honey ring compound preparation are improved, and the security and the effectiveness of drugs used by people are guaranteed.
Description
Technical field
The present invention relates to the quality determining method of medicine, be specifically related to ginkgo honey ring compound preparation quality determining method, especially adopt thin-layered chromatography to differentiate the halimasch powder, adopt the quality determining method of the content of HPLC Determination of Adenosine.
Background technology
Ginkgo honey ring compound preparation is the focus active substance ginkgo biloba p.e of selecting natural plant research in modern age, carry out scientific composition with the effective ingredient of China traditional Chinese medicine armillaria mellea accreting with Rhizoma Gastrodiae, the compound preparation that uses modern preparation process to make, at present domestic only have ginkgo honey collar extension to take a kind of formulation listing of solution production and sales.
Ginkgo leaf is a kind of plant with very high medical value, ginkgo is one of ancient seeds of China, and life on earth is gone through the change in 100000000000 years, especially after the glacier covering of the 4th century, only have ginkgo still to keep its most original looks, be called as " living fossil " in the organic evolution history.Ginkgo leaf record in the past book on Chinese herbal medicine and so on medicine book is less, until the thirties in 20th century, Japan and West Germany have just begun the research of ginkgo leaf.Along with deepening continuously of modern pharmacological research, to find not only to contain Flavonoid substances in the ginkgo leaf, and also have the compounds such as terpene lactones, phenols, the pharmacological action of their brilliances has been familiar with gradually by people, and clinical application range progressively enlarges.
The effect of ginkgo biloba p.e in human body, mainly be to strengthen antiotasis, coronary artery dilator, softening blood vessel, improve vasopermeability, reduce blood pressure, reduce blood fat and cholesterol, anti-platelet aggregation, minimizing thrombosis, reduce endovascular HDL-C (HDL-C), triglyceride (TG), thereby reach hypotensive, reducing blood lipid, fall the sticking effect of blood.
Modern study shows that ginkgo leaf contains flavones ingredient ginkegetin (ginkgetin), Isoginkgetin (isoginkgetin), demethyl ginkegetin (bilobetin), rutin, Kaempferide-3-scillabiose, Kaempferide, Quercetin, Isorhamnetin (isorhamnetin) etc.; Other contains bitter principle ginkgo three lactone A (ginkgolideA), B, C and the new lactone A of ginkgo (bilobalide A); Acids composition shihimic acid (shikimic acid), D-saccharic acid (D-glucaric acid), ginkgolic acid (ginkgolic acid). still contain gingko alcohol (ginnol), bilobanone (ginnone), nonacosane, Octacosanol, hexenal, cupreol, stigmasterol and vitamin etc.
More deep to the qualitative and quantitative detection research of ginkgo biloba p.e both at home and abroad at present, in " Pharmacopoeia of People's Republic of China 2010 editions " ginkgo biloba p.e standard, existing qualitative discrimination method also has two method for quantitatively determining of total flavonoids and terpene lactone.
The genus of Armillaria Basidiomycetes Agaricales fungi is the indispensable mutualistic symbiosis bacterium of rhizoma Gastrodiae.Halimasch distributes very wide, and most domestic provinces and cities all have.Halimasch is nutritious, also has medical value.It is reported, dried mushroom contains crude protein 11.4%,
Fat 5.2%, carbohydrates 75.9%, cellulose 5.8%, ash content 7.5%, 384 kilocalories of heats.The solid fermentation goods of halimasch can replace rhizoma Gastrodiae to be used as medicine, the diseases such as hypertension VBI, Meniere's syndrome, vegetative nerve functional disturbance are caused dizzy patient, result for the treatment of is better, and limb fiber crops, insomnia, tinnitus, apoplexy sequelae etc. are also had certain curative effect.
At present ginkgo biloba p.e is compared in the research of halimasch chemical composition and will be fallen behind a lot, mainly concentrate on fat-soluble sequiterpene aromatic esters compounds and water miscible halimasch intracellular polyse constituents.Because chemical constitution study is weak, so to the qualitative and quantitative detection research of halimasch just still less, research few in number all is the liposoluble constituents such as ligroin extraction that concentrate on halimasch, does not then have the method for qualitative and quantitative detection of specificity for the halimasch water soluble ingredient
At present unique ginkgo honey collar extension of getting permission to go on the market takes solution, and this target level of product quality is recorded in the 16 of State Food and Drug Administration's " national drug standards-chemicals provincial standard rising national standard ", standard No. WS
1-XG-004-2001.The thin-layer identification method of ginkgo biloba p.e and the content assaying method of ginkgo leaf total flavonoid alcohol glycosides are only arranged in this standard, the qualitative discriminating project and the assay project that lack halimasch, can not reflect whether product contains the content of halimasch in halimasch effective constituent and the product, can't effectively detect the quality of formulation products.
Summary of the invention
Owing among the ginkgo honey ring compound preparation preparation technology, halimasch is adopted aqueous extraction-alcohol precipitation technology, so substantially do not contain the liposoluble constituent such as halimasch sequiterpene aromatic esters compounds in the said preparation, do not have the polysaccharide composition yet.The inventor is through great many of experiments, overcome deficiency of the prior art, worked out the method for qualitative and quantitative detection for the halimasch water soluble ingredient in the ginkgo honey ring compound preparation, namely adopted thin-layered chromatography to differentiate in the ginkgo honey ring compound preparation and contain the halimasch powder; Adopt the content of adenosine in the high effective liquid chromatography for measuring ginkgo honey ring compound preparation.
Thin-layered chromatography differentiates that the condition that contains the halimasch powder in the ginkgo honey ring preparation is:
Chromatographic condition: thin layer plate silica G
Developping agent normal butyl alcohol-acetic acid-water (4: 1: 1～7: 1: 1)
The developer ethanol solution of ninhydrin
The preparation of reference substance solution: get the halimasch control medicinal material and add water, boil, keep little boiling, filter, filtrate evaporate to dryness, residue add Diluted Alcohol dissolving, in contrast medicinal material solution;
The preparation of need testing solution: get this product, add the second alcohol and water, ultrasonic processing filters, and filtrate evaporate to dryness, residue add the Diluted Alcohol dissolving, as need testing solution;
Discrimination method: draw respectively reference substance solution and need testing solution, put respectively on silica gel g thin-layer plate, take normal butyl alcohol-acetic acid-water (4: 1: 1～7: 1: 1) as developping agent, launch, take out, dry, spray is heated to the spot colour developing at 105 ℃ clear with ethanol solution of ninhydrin; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.Studies show that ginkgo biloba p.e is to the method result that is negative.
The content of adenosine in the high effective liquid chromatography for measuring ginkgo honey ring compound preparation, its condition is:
Chromatographic condition: take octadecylsilane chemically bonded silica as filling agent;
Take acetonitrile: water (6: 94) is as mobile phase;
The detection wavelength is 260nm;
Theoretical cam curve is calculated by the adenosine peak should be not less than 2500;
It is an amount of that the preparation precision of reference substance solution takes by weighing the adenosine reference substance, adds water and make the solution that every 1mL contains 0.05mg;
The preparation of need testing solution:
(1) ginkgo honey ring capsule: get this product content, porphyrize is got powder, accurately weighed, put in the tool plug conical flask accurate 50% methanol solution that adds, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, weighed weight is again supplied the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(2) ginkgo honey ring plate: get this product, porphyrize is got powder, accurately weighed, put in the tool plug conical flask accurate 50% methanol solution that adds, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, weighed weight is again supplied the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(3) ginkgo honey ring particle: get this product, porphyrize is got powder, accurately weighed, put in the tool plug conical flask accurate 50% methanol solution that adds, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, weighed weight is again supplied the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(4) ginkgo honey collar extension takes solution: get this product, shake up, filter, get subsequent filtrate as need testing solution.
Determination method: precision is drawn reference substance solution and each 20uL of need testing solution respectively, injects high performance liquid chromatograph, measures, by the content of external standard method calculating adenosine.
Ginkgo honey of the present invention encircles the quality determining method of compound preparation, the halimasch composition in the ginkgo honey ring compound preparation has been carried out the qualitative and quantitative detection of specificity, can effectively reflect the content that whether contains halimasch in halimasch and the product in the product.In act.std, increase quality determining method of the present invention, improved specificity and the reliability of ginkgo honey ring compound preparation drug quality detection method, guaranteed security and the validity of people's medication.
Embodiment
The present invention is further elaborated below in conjunction with embodiment, but the present invention is not had any restriction.
Embodiment 1: thin-layered chromatography is differentiated in the ginkgo honey ring capsule and is contained halimasch
The preparation of control medicinal material solution: get halimasch control medicinal material 1g, accurately weighed, add water 50ml, boil and keep little and boiled 30 minutes, filter, filtrate evaporate to dryness, residue add Diluted Alcohol 2ml dissolving, in contrast medicinal material solution;
The preparation of need testing solution: get this product content 0.5g, accurately weighed, put in the tool plug conical flask, add Diluted Alcohol 10ml, close plug, ultrasonic processing (power 250W, frequency 25kHz) 30 minutes filters, filtrate evaporate to dryness, residue add Diluted Alcohol 2ml dissolving, as need testing solution;
According to thin-layered chromatography (two appendix V of Chinese Pharmacopoeia B) test, draw mentioned solution 5 μ l, point sample is on the silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take normal butyl alcohol-acetic acid-water (7: 1: 1) as developping agent, launch, take out, dry, spray is with 0.2% ethanol solution of ninhydrin, 105 ℃ of heating 15 minutes, inspect immediately, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.
Embodiment 2: the content of adenosine in the high effective liquid chromatography for measuring ginkgo honey ring capsule
1 instrument
1.1 high performance liquid chromatograph
1.2 chromatographic column
Octadecylsilane chemically bonded silica is filling agent, and theoretical cam curve is calculated by the adenosine peak should be not less than 2500.
1.3 ultraviolet absorption detector
2 chromatographic conditions
2.1 mobile phase: 6% acetonitrile: water
2.2 detection wavelength: 260nm
2.3 column temperature: room temperature
2.4 flow velocity: 1.0ml/min
The preparation of 3 samples
3.1 the preparation of contrast solution
It is an amount of that precision takes by weighing the adenosine reference substance, adds water and make the solution that every 1mL contains 0.05mg.
3.2 the preparation of need testing solution
(1) capsule
Get 20 of this product, porphyrize is got approximately 1.3g of powder, accurately weighed, put in the tool plug conical flask the accurate 50% methanol solution 25ml that adds, close plug, weighed weight, ultrasonic processing (power 250W, frequency 25kHz) 30 minutes, lets cool, more weighed weight, supply the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(2) halimasch medicinal material
Get approximately 2.6g of halimasch powder, accurately weighed, put in the tool plug conical flask, accurate 50% methanol solution 25ml, close plug, the weighed weight of adding, ultrasonic processing (power 250W, frequency 25kHz) 30 minutes, lets cool, more weighed weight, supply the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(3) blank solution
Get the preparation that does not contain halimasch blank, press the preparation of need testing solution operation steps, get subsequent filtrate as blank solution.
4 operation stepss
(1) the accurate blank of drawing is disturbed solution 20uL, injects high performance liquid chromatograph, and the result shows: blank solution is measured noiseless to adenosine.
(2) precision is drawn reference substance solution and each 20uL of need testing solution respectively, injects high performance liquid chromatograph, measures, by the content of external standard method calculating adenosine.
Claims (2)
1. the quality determining method of ginkgo honey ring compound preparation is characterized in that adopting thin-layered chromatography, differentiates in the ginkgo honey ring compound preparation to contain the halimasch powder, and operation steps is as follows:
Chromatographic condition: thin layer plate silica G
Developping agent normal butyl alcohol-acetic acid-water (4: 1: 1～7: 1: 1)
The developer ethanol solution of ninhydrin
The preparation of reference substance solution: get the halimasch control medicinal material and add water, boil, keep little boiling, filter, filtrate evaporate to dryness, residue add Diluted Alcohol dissolving, in contrast medicinal material solution;
The preparation of need testing solution: get this product, add the second alcohol and water, ultrasonic processing filters, and filtrate evaporate to dryness, residue add the Diluted Alcohol dissolving, as need testing solution;
Discrimination method: draw respectively reference substance solution and need testing solution, put respectively on silica gel g thin-layer plate, take normal butyl alcohol-acetic acid-water (4: 1: 1～7: 1: 1) as developping agent, launch, take out, dry, spray is heated to the spot colour developing at 105 ℃ clear with ethanol solution of ninhydrin; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the principal spot of aobvious same color.
2. the quality determining method of ginkgo honey ring compound preparation is characterized in that adopting high effective liquid chromatography for measuring ginkgo honey to encircle the content of adenosine in the compound preparation, and operation steps is as follows:
Chromatographic condition: take octadecylsilane chemically bonded silica as filling agent;
Take acetonitrile: water (6: 94) is as mobile phase;
The detection wavelength is 260nm;
Theoretical cam curve is calculated by the adenosine peak should be not less than 2500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the adenosine reference substance, adds water and make the solution that every 1mL contains 0.05mg;
The preparation of need testing solution:
(1) ginkgo honey ring capsule: get this product content, porphyrize is got powder, accurately weighed, put in the tool plug conical flask accurate 50% methanol solution that adds, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, weighed weight is again supplied the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(2) ginkgo honey ring plate: get this product, porphyrize is got powder, accurately weighed, put in the tool plug conical flask accurate 50% methanol solution that adds, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, weighed weight is again supplied the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(3) ginkgo honey ring particle: get this product, porphyrize is got powder, accurately weighed, put in the tool plug conical flask accurate 50% methanol solution that adds, close plug, weighed weight, ultrasonic processing 30 minutes, let cool, weighed weight is again supplied the weight of less loss with 50% methanol solution, shake up, filter, get subsequent filtrate as need testing solution.
(4) ginkgo honey collar extension takes solution: get this product, shake up, filter, get subsequent filtrate as need testing solution.
Determination method: precision is drawn reference substance solution and each 20uL of need testing solution respectively, injects high performance liquid chromatograph, measures, by the content of external standard method calculating adenosine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892686A (en) * | 2015-05-27 | 2015-09-09 | 中国科学院西北高原生物研究所 | Method for separating and purifying armillaria luteo-virens entity nucleoside compound |
| CN113567593A (en) * | 2021-09-01 | 2021-10-29 | 邛崃天银制药有限公司 | Ginkgo honey ring oral solution multi-component content detection and fingerprint spectrum method construction thereof |
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| US20110262561A1 (en) * | 2010-04-26 | 2011-10-27 | National Research Institute Of Chinese Medicine | Protoilludance Norsesquiterpenoid Esters and Uses Thereof |
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- 2012-04-05 CN CN2012100967063A patent/CN103364520A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110262561A1 (en) * | 2010-04-26 | 2011-10-27 | National Research Institute Of Chinese Medicine | Protoilludance Norsesquiterpenoid Esters and Uses Thereof |
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| 中华人民共和国卫生部药典委员会: "《药品标准 中药成方制剂 第十九册》", 31 December 1998 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892686A (en) * | 2015-05-27 | 2015-09-09 | 中国科学院西北高原生物研究所 | Method for separating and purifying armillaria luteo-virens entity nucleoside compound |
| CN113567593A (en) * | 2021-09-01 | 2021-10-29 | 邛崃天银制药有限公司 | Ginkgo honey ring oral solution multi-component content detection and fingerprint spectrum method construction thereof |
| CN113567593B (en) * | 2021-09-01 | 2023-02-03 | 邛崃天银制药有限公司 | Ginkgo honey ring oral solution multi-component content detection and fingerprint spectrum method construction thereof |
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Application publication date: 20131023 |