CN1570625A - Detection method for toxicological harmless traditional Chinese herbal Asarum - Google Patents
Detection method for toxicological harmless traditional Chinese herbal Asarum Download PDFInfo
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- CN1570625A CN1570625A CN 200410020473 CN200410020473A CN1570625A CN 1570625 A CN1570625 A CN 1570625A CN 200410020473 CN200410020473 CN 200410020473 CN 200410020473 A CN200410020473 A CN 200410020473A CN 1570625 A CN1570625 A CN 1570625A
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- aristolochic acid
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Abstract
This invention publics a detecting method about a nontoxic traditional medicine liao asarum. It is to extract volatile oil according to a method of volatile oil extraction from Chinese pharmacopeia, the 2000 edition, dissolve by cyclohexane, and inject it into gas-chromatograph-mass spectrometer to draft fingerprint pattern. Through the analysis result by computer, it is to get 28-wave crest, such as methyleugenol, safrole myristicin and so on, where the essential component methyleugenol is about 37 percent. The volatile oil extracted according to pharmacopeia is dissolved by acetic ester, added methyl alcohol, and injected into high efficiency liquid chromatography to get high efficiency liquid fingerprint pattern. It is to adopt liquid hypersonic extracted for 30 minutes by methyl alcohol-water (3:1) ,and inject it into high efficiency liquid chromatography to build detecting method about high efficiency liquid chromatogram for aristolochic acid.
Description
Technical field:
The present invention relates to medical technical field, it relates to the nonhazardous Chinese crude drug HERBA ASARI from Liaoning of China detection method that can expect Chinese crude drug GAP research, determines the method for quality control of the HERBA ASARI from Liaoning of China of no aristolochic acid in definite saying.
Background technology:
HERBA ASARI from Liaoning of China is a conventional Chinese medicine, and each edition pharmacopeia is all on the books, the main product the Northeast, and the product person is the best in quality with Liaoning, does not contain aristolochic acid, so have won fame both at home and abroad, claims HERBA ASARI from Liaoning of China.The former plant of HERBA ASARI from Liaoning of China is root of Chinese wild ginger Asarumheterotropoides Fr. Schmidt var.mandxhuricum (Maxim) Kitag. and Seoul root of Chinese wild ginger Asarum sieboldii Miq.Var.seoulense Nakai. tool expelling wind and clearing away cold, understand things pain-stopping, the warming lung to reduce watery phlegm effect, its main pharmacodynamics composition is a volatile oil, has pharmacological actions such as analgesic, analgesia, calm, anticonvulsion, anesthesia.
Chinese material medicine resource has stronger region than other biological resource, so traditional Chinese medicine should be selected genunie medicinal materials for use when emphasizing to use Chinese medicine always.Genunie medicinal materials are meant the medicinal material that is produced in the region of specific natural conditions, ecologic environment, its production is comparatively concentrated, cultivation technique, gather, process certain being particular about also all arranged, than other area good, good effects of medical material quanlity of the same race of producing.HERBA ASARI from Liaoning of China beginning is stated from Shennong's Herbal, classifies as top gradely, and Tao Hongjing claims that " the present with the Dongyang person's of bordering on the sea shape section is too late Koryo, Huayin person of Xin Lie." Koryo (modern Benxi, Huan's benevolence one band) HERBA ASARI from Liaoning of China place of production unanimity up to the present.Modern study shows that the effective constituent of the root of Chinese wild ginger is volatile oil, mainly contains methyl eugenol, safrole and elemicine in the volatile oil, and produce in summation Liaoning of volatile oil content is 2.92%, and the magnificent root of Chinese wild ginger is 2.68%.So it is best that root of Chinese wild ginger quality is produced in Liaoning, drug effect the best.Liaoning is its genuine producing region, so have won fame both at home and abroad.Just seem very important but how HERBA ASARI from Liaoning of China is detected, still do not have normalized detection method at present.
Summary of the invention:
The object of the present invention is to provide the detection method of the nonhazardous Chinese crude drug HERBA ASARI from Liaoning of China of GAP.Characteristics of the present invention are to adopt high performance liquid chromatogram, gas chromatography to carry out assay the Chinese medicine HERBA ASARI from Liaoning of China, formulate the detection method of finger-print and definite aristolochic acid.
The detection method of above-mentioned Chinese medicine HERBA ASARI from Liaoning of China is provided, and its feature mainly comprises: the formulation of high performance liquid chromatogram, gas-phase fingerprint pattern is practical; The detection method of aristolochic acid is easy, accurate.
The detection method of above-mentioned Chinese medicine HERBA ASARI from Liaoning of China is provided, comprising;
A: the vapor detection method of volatile oil.Adopt " volatile oil extraction method an extraction of Chinese pharmacopoeia version in 2000 volatile oil, dissolve through cyclohexane, in injection gas chromatography-mass spectrometry chromatogram view, draw finger-print, and formulation quality standard, the machine analysis result obtains 28 peaks such as methyl eugenol, safrole, myristicin as calculated, and wherein the principal ingredient methyl eugenol accounts for 37%.
B: the highly effective liquid phase chromatography detection method of volatile oil.Through the pharmacopeia method extract the volatile oil make with a spot of acetic acid ethyl dissolution after, add methyl alcohol, inject high-efficient liquid phase chromatogram discuss, obtain high-efficiency liquid-phase fingerprint, and the formulation quality standard.
C: the detection method of aristolochic acid.Aristolochic acid is one of material that causes injury of kidney, must study aristolochic acid, adopts 30 minutes solution of methanol-water (3: 1) ultrasonic Extraction as test liquid, injects high performance liquid chromatograph, sets up the detection method of high performance liquid chromatography aristolochic acid.
Advantage of the present invention is: the detection method that the nonhazardous Chinese crude drug HERBA ASARI from Liaoning of China of GAP is provided.Quality for the nonhazardous Chinese crude drug HERBA ASARI from Liaoning of China of determining GAP provides assurance.Formulated the detection method of practicable aristolochic acid.
Description of drawings:
Fig. 1 is the gas-phase fingerprint pattern of the root of Chinese wild ginger.
Fig. 2 is the high-efficiency liquid-phase fingerprint of the root of Chinese wild ginger.
Fig. 3 is an aristolochic acid controlling chart in the root of Chinese wild ginger leaf.
Fig. 4 is an aristolochic acid controlling chart in the root of Chinese wild ginger stem.
Fig. 5 is an aristolochic acid controlling chart in the Radix Asari.
Fig. 6 is the limit examine figure of aristolochic acid.
Fig. 7 is 10 times of spirograms of limit examine of aristolochic acid.
Embodiment:
Embodiment 1:
The vapor detection method of volatile oil.
Get the root of Chinese wild ginger 100g of 60 ℃ of dryings, put in the 1000ml flask, add water 600ml, soaked overnight, by " one one of Chinese pharmacopoeia version in 2000 is extracted 8 hours volatile oil and collected the volatile oil that obtains and put the 10ml measuring bottle, adds cyclohexane and dissolves and be diluted to scale, get 0.4 μ l and inject gas phase-mass spectrometry chromatograph, chromatographic condition is:
U.S. Finigan Trace GC-MS instrument, DB-1MS (0.25 * 0.25 * 30) temperature programme: initial temperature is 60 ℃, keep that the speed of 10 ℃/min rises to 230 ℃ after 3 minutes, keep 20min, the vaporizer temperature: 260 ℃, split ratio: 10: 1, carrier gas: He, flow velocity: 1ml/min, sample size: 0.4 μ l, electron bombard (EI) ion flow, high sub-energy 70ev, the ion flow temperature: 230 ℃, mass scanning scope: 33u-500u, sweep speed: 1000amu/s, write down 40 minutes chromatogram, with 10 batches of roots of Chinese wild ginger is research object, gets the gas-phase fingerprint pattern of volatile oil, and formulates quality standard.1. thujenes wherein; 2. australene; 3. amphene; 4. α-terpinene; 5. nopinene; 6. myrcene; 7. α-phellandrene; 8.3-carene; 9. right-poly-umbrella flower is; 10. hesperidene; 11. γ-Song Youxi; 12. α-terpinolene; 13. Eucarvone; 14. borneol; 15. like the leather brain; 16.3, the 5-dimethoxy-p; 17. safrole; 18. methyl eugenol; 19. trimethoxytoluene; 20. β-gurjunene; 21. α-guaiene; 22. β-guaiene; 23. myristicin; 24. δ Cadinene; 25.asarone; 26. it is trans-isoelemicine; 27. it is different-isoelemicine.
Wherein the 3-carene has local irritant effect, and Eucarvone has the antitussive and antiasthmatic effect, and methyl eugenol has the spasmolysis cooling effect.
Embodiment 2:
The highly effective liquid phase chromatography detection method of volatile oil.
The accurate 0.2ml of absorption of volatile oil that extracts is put in the 10ml measuring bottle, add acetic acid ethyl dissolution and be diluted to scale, get 10 μ l and inject high performance liquid chromatograph, chromatographic condition is:
Day island proper Tianjin LC-10AT of company chromatograph, Tianjin, island SPD-10A type ultraviolet-visible detecting device.Dalian is according to the sharp peculiar limit Kromasil C18 (200mm * 4.6mm of company, 5 μ m) chromatographic column, second eyeball-water (40-60) is moving phase, flow velocity 0.8ml/min, wavelength 250nm, writing down 50 minutes chromatograms, is research object with 10 batches of roots of Chinese wild ginger, gets the high-efficiency liquid-phase fingerprint of volatile oil and formulates quality standard.
Embodiment 3:
The detection method of aristolochic acid.
Asarum medicinal materials root, stem, each 1g of leaf powder are got in the preparation of need testing solution, add methanol-water (3: 1) solution 25ml, soak 15min, and sonicated 20min filters.Filtrate filters with 0.45 μ m miillpore filter again, promptly gets need testing solution.
The preparation aristolochic acid reference substance of reference substance solution becomes the solution of 0.45 μ g/ml with methanol-water (3: 1) solution dilution, shakes up, and promptly gets reference substance solution.
Get each 10 μ l of above-mentioned need testing solution and reference substance solution, inject HPLC.
Day island proper Tianjin LC-10AT of company chromatograph, Tianjin, island SPD-10A type ultraviolet-visible detecting device, Dalian is according to the sharp peculiar limit Kromasil C18 (200mm * 4.6mm of company, 5 μ m) chromatographic column, moving phase: 0.05mol/L sodium dihydrogen phosphate (phosphoric acid 1ml/L)-acetonitrile (60: 40), flow velocity: 1ml/min, detect wavelength: 400nm, column temperature: room temperature, sample size: 10 μ l, the theoretical cam curve of aristolochic acid does not hang down 4900.The aristolochic acid reference substance range of linearity and lowest detectable limit test aristolochic acid reference substance becomes the solution of 0.09mg/ml with methanol-water (3: 1) dissolving and solution dilution, shakes up, and dilutes again, shake up, accurately draw 10 μ l, inject HPLC, record the range of linearity: 45-900 μ g.Signal to noise ratio (S/N ratio) is 3: 1 o'clock, and aristolochic acid reference substance minimal detectable concentration is 0.45 μ g/ml, and limit of identification is 4.5ng.
All do not have chromatographic peak in the high-efficient liquid phase chromatogram of the root of Chinese wild ginger in above-mentioned source on corresponding position, aristolochic acid standard items peak, showing does not have aristolochic acid in the root of Chinese wild ginger.
Claims (1)
1. the detection method of nonhazardous Chinese crude drug HERBA ASARI from Liaoning of China is characterized in that:
A: the vapor detection method of volatile oil; Adopt " volatile oil extraction method an extraction of Chinese pharmacopoeia version in 2000 volatile oil, dissolve through thiacyclohexane, in injection gas chromatography-mass spectrometry chromatogram view, draw finger-print, and formulation quality standard, the machine analysis result obtains 28 peaks such as methyl eugenol, safrole, myristicin as calculated, and wherein the principal ingredient methyl eugenol accounts for 37%;
B: the highly effective liquid phase chromatography detection method of volatile oil: through the pharmacopeia method extract the volatile oil make with a spot of acetic acid ethyl dissolution after, add methyl alcohol, the injection high-efficient liquid phase chromatogram discuss obtains high-efficiency liquid-phase fingerprint;
C: the detection method of aristolochic acid: adopt 30 minutes solution of methanol-water (3: 1) ultrasonic Extraction as test liquid, inject high performance liquid chromatograph, set up the detection method of high performance liquid chromatography aristolochic acid.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313139C (en) * | 2005-08-31 | 2007-05-02 | 通化东宝药业股份有限公司 | Method for preparing medicine for treating angioneurotic headache |
| CN100392397C (en) * | 2005-12-28 | 2008-06-04 | 劲牌有限公司 | Method for checking clove medicinal material by using traditional medicine fingerprint pattern technology |
| CN1847841B (en) * | 2005-04-12 | 2010-04-28 | 天津天士力制药股份有限公司 | Method of detecting content of micro amount of aristolochic acid A in water extract of Chinese medicine |
| CN101455695B (en) * | 2007-12-11 | 2012-10-03 | 广西壮族自治区花红药业股份有限公司 | Quality control method of aristolochic acid A in Asarum medicinal materials and repellent-antalgesic tincture |
| CN104090041A (en) * | 2014-07-15 | 2014-10-08 | 中山大学 | Method for detecting content of methyleugenol in melaleuca bracteata volatile oil |
| CN105388231A (en) * | 2015-12-29 | 2016-03-09 | 成都普思生物科技股份有限公司 | Method for detecting purity of elemicin |
| CN106198838A (en) * | 2016-07-04 | 2016-12-07 | 江西天施康中药股份有限公司 | A kind of detection method of bupleurum root and asarum herb injection |
| CN109030702A (en) * | 2018-11-03 | 2018-12-18 | 青海瑞成药业(集团)有限公司 | A kind of quality determining method that blood stasis-eliminating and stagnation-dissipating enema is new |
| CN110702808A (en) * | 2019-09-25 | 2020-01-17 | 中国兽医药品监察所 | Quality inspection method of radix bupleuri and asarum in chaihin injection |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086720A (en) * | 1992-11-09 | 1994-05-18 | 肖维益 | Prescription of a kind of carsick medicine for external use and preparation method thereof |
| CN1096447A (en) * | 1993-06-18 | 1994-12-21 | 乔振纲 | Health mask specially for tracheitis patient and pharmaceutical formulation thereof |
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2004
- 2004-04-27 CN CNB2004100204734A patent/CN100422734C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1847841B (en) * | 2005-04-12 | 2010-04-28 | 天津天士力制药股份有限公司 | Method of detecting content of micro amount of aristolochic acid A in water extract of Chinese medicine |
| CN1313139C (en) * | 2005-08-31 | 2007-05-02 | 通化东宝药业股份有限公司 | Method for preparing medicine for treating angioneurotic headache |
| CN100392397C (en) * | 2005-12-28 | 2008-06-04 | 劲牌有限公司 | Method for checking clove medicinal material by using traditional medicine fingerprint pattern technology |
| CN101455695B (en) * | 2007-12-11 | 2012-10-03 | 广西壮族自治区花红药业股份有限公司 | Quality control method of aristolochic acid A in Asarum medicinal materials and repellent-antalgesic tincture |
| CN104090041A (en) * | 2014-07-15 | 2014-10-08 | 中山大学 | Method for detecting content of methyleugenol in melaleuca bracteata volatile oil |
| CN105388231A (en) * | 2015-12-29 | 2016-03-09 | 成都普思生物科技股份有限公司 | Method for detecting purity of elemicin |
| CN106198838A (en) * | 2016-07-04 | 2016-12-07 | 江西天施康中药股份有限公司 | A kind of detection method of bupleurum root and asarum herb injection |
| CN106198838B (en) * | 2016-07-04 | 2017-08-15 | 江西天施康中药股份有限公司 | A kind of detection method of bupleurum root and asarum herb parenteral solution |
| CN109030702A (en) * | 2018-11-03 | 2018-12-18 | 青海瑞成药业(集团)有限公司 | A kind of quality determining method that blood stasis-eliminating and stagnation-dissipating enema is new |
| CN110702808A (en) * | 2019-09-25 | 2020-01-17 | 中国兽医药品监察所 | Quality inspection method of radix bupleuri and asarum in chaihin injection |
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| CN100422734C (en) | 2008-10-01 |
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Granted publication date: 20081001 Termination date: 20110427 |