Detection method for toxicological harmless traditional Chinese herbal Asarum

A detection method and technology of Chinese herbal medicines, applied in the field of medicine, can solve problems such as non-standardized detection methods

Inactive Publication Date: 2005-01-26
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, how to detect Liaoshixin is very important, a

Method used

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  • Detection method for toxicological harmless traditional Chinese herbal Asarum
  • Detection method for toxicological harmless traditional Chinese herbal Asarum
  • Detection method for toxicological harmless traditional Chinese herbal Asarum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Gas phase detection of volatile oils.

[0020] Take 100g of asarum dried at 60°C, put it in a 1000ml flask, add 600ml of water, soak overnight, extract the volatile oil collected for 8 hours according to Part 1 of "Chinese Pharmacopoeia" 2000 edition, put the collected volatile oil in a 10ml measuring bottle, add cyclohexane to dissolve and dilute To the scale, take 0.4 μl and inject it into the gas phase-mass spectrometer, the chromatographic conditions are:

[0021] US Finigan Trace GC-MS instrument, DB-1MS (0.25×0.25×30) temperature program: the initial temperature is 60°C, keep it for 3 minutes, then rise to 230°C at a rate of 10°C / min, keep it for 20min, the temperature of the vaporization chamber: 260°C, split ratio: 10:1, carrier gas: He, flow rate: 1ml / min, injection volume: 0.4μl, electron bombardment (EI) ion flow, high son energy 70ev, ion flow temperature: 230°C, mass scanning Range: 33u-500u, scan rate: 1000amu / s, record chromatograms for 40 minutes, take ...

Embodiment 2

[0024] High performance liquid chromatography detection of volatile oils.

[0025] Accurately draw 0.2ml of the extracted volatile oil, put it in a 10ml measuring bottle, add ethyl acetate to dissolve and dilute to the mark, take 10μl and inject it into a high performance liquid chromatograph, the chromatographic conditions are:

[0026] Shimadzu Corporation LC-10AT chromatograph, Shimadzu SPD-10A UV-visible detector. Dalian Elite Co., Ltd. Kromasil C18 (200mm×4.6mm, 5μm) chromatographic column, acetonitrile-water (40-60) as mobile phase, flow rate 0.8ml / min, wavelength 250nm, record chromatograms for 50 minutes, and use 10 batches of fine Xin was the research object, and the HPLC fingerprint of the volatile oil was obtained and the quality standard was formulated.

Embodiment 3

[0028] Method for the detection of aristolochic acid.

[0029] Preparation of the test solution Take 1g each of Asarum root, stem and leaf powder, add 25ml of methanol-water (3:1) solution, soak for 15min, sonicate for 20min, and filter. The filtrate was filtered through a 0.45 μm microporous membrane to obtain the test solution.

[0030] Preparation of reference substance solution Aristolochic acid reference substance was diluted with methanol-water (3:1) solution to a 0.45 μg / ml solution, and shaken to obtain the reference substance solution.

[0031] Take 10 μl each of the above-mentioned test solution and reference solution, and inject them into HPLC.

[0032] Shimadzu Corporation LC-10AT chromatograph, Shimadzu SPD-10A UV-visible detector, Dalian Elite Co., Ltd. Kromasil C18 (200mm×4.6mm, 5μm) chromatographic column, mobile phase: 0.05mol / L dihydrogen phosphate Sodium (containing phosphoric acid 1ml / L)-acetonitrile (60:40), flow rate: 1ml / min, detection wavelength: 400n...

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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: [0001] The invention relates to the technical field of medicine, specifically, it relates to a detection method of the non-toxic Chinese medicinal material Liaoshixin which can be expected to be studied in standardized planting of Chinese medicinal materials, and a quality control method for determining the quality of Liaoxixin without aristolochic acid. Background technique: [0002] Liaoshixin is a commonly used traditional Chinese medicine, which is recorded in various editions of the Pharmacopoeia. It is mainly produced in the Northeast region. The quality of Liaoning products is the best, and it does not contain aristolochic acid. Therefore, it is well-known both at home and abroad. The original plants of Liao Asarum are Asarum heterotropoides Fr. Schmidt var.mandxhuricum (Maxim) Kitag. and Asarum sieboldii Miq.Var. seoulense Nakai. The active ingredient is volatile oil, which has pharmacological effects such as antipyretic, analgesic, sedative, anticon...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 孙启时贾凌云
Owner SHENYANG PHARMA UNIVERSITY
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