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Detection method of content of wild baicalin in traditional Chinese medicine

A detection method and scutellarin technology are applied in the field of quality control of traditional Chinese medicinal materials, and can solve the problems of insufficient peak purity of scutellarin, complicated and time-consuming pretreatment of medicinal materials, poor adaptability and the like, and achieve simple and convenient processing and long processing time. , the effect of strong adaptability

Inactive Publication Date: 2019-03-15
YUNNAN BIOVALLEY PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The method for determining the content of Erigeron breviscapus recorded in the 2015 edition of "Chinese Pharmacopoeia" is complicated and time-consuming for the pretreatment of medicinal materials, and chloroform with strong hepatotoxicity is used for reflux extraction. Repeated verifications found that the purity of the scutellarin peak was not enough, and it contained the peak of another substance scutellarin, so the content determined by this would be falsely high, see the content of the invention for details

Method used

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  • Detection method of content of wild baicalin in traditional Chinese medicine
  • Detection method of content of wild baicalin in traditional Chinese medicine
  • Detection method of content of wild baicalin in traditional Chinese medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] experiment procedure:

[0084] (1) Preparation of reference substance solution: take an appropriate amount of scutellarin reference substance, weigh it accurately, add ethanol to make a solution containing 0.1mg per 1ml

[0085] (2) Preparation of the test solution: take 1.0 g of Erigeron breviscapus coarse powder, accurately weigh it, put it in a stoppered Erlenmeyer flask, accurately add 100 ml of 50% ethanol solution, weigh it, ultrasonically treat it for 1 hour, and seal it tightly. , weigh again, make up the lost weight with 50% ethanol solution, shake well, filter with a 0.45um filter head, and take the continued filtrate

[0086] (3) Chromatographic conditions and system suitability test: chromatographic column Inertsil ODS-3 5μm 4.6×250mm; mobile phase: tetrahydrofuran: acetonitrile: 0.2% phosphoric acid solution: (14:7:79); column temperature: 30°C; The flow rate is 0.8ml / min, the detection wavelength is 335nm; the number of theoretical plates is not less than...

Embodiment 2

[0090] experiment procedure:

[0091] (1) Preparation of reference substance solution: take an appropriate amount of scutellarin reference substance, weigh it accurately, add ethanol to make a solution containing 0.1mg per 1ml

[0092] (2) Preparation of the test solution: take 1.0 g of Erigeron breviscapus coarse powder, accurately weigh it, put it in a stoppered Erlenmeyer flask, accurately add 100 ml of 75% ethanol solution, weigh it, ultrasonically treat it for 1 hour, and seal it tightly. , weigh again, make up the lost weight with 75% ethanol solution, shake well, filter with a 0.45um filter head, and take the continued filtrate

[0093] (3) Chromatographic conditions and system suitability test: Welch XB-C18 chromatographic column 5μm 4.6×250mm; mobile phase: tetrahydrofuran: acetonitrile: 0.2% phosphoric acid solution: (14:7:79); column temperature: 35°C; The flow rate is 1.0ml / min, the detection wavelength is 335nm; the number of theoretical plates is not less than 5...

Embodiment 3

[0097] experiment procedure:

[0098] (1) Preparation of reference substance solution: Take an appropriate amount of scutellarin reference substance, weigh it accurately, add ethanol to make a solution containing 0.1mg per 1ml.

[0099] (2) Preparation of the test solution: take 1.0 g of Erigeron breviscapus coarse powder, accurately weigh it, put it in a stoppered Erlenmeyer flask, accurately add 100 ml of 50% ethanol solution, weigh it, ultrasonically treat it for 1 hour, and seal it tightly. , weigh again, make up the lost weight with 50% ethanol solution, shake well, filter with a 0.45um filter head, and take the continued filtrate

[0100] (3) Chromatographic conditions and system suitability test: Agilent ZORBAX SB-C18 chromatographic column 5μm 4.6×250mm; mobile phase: tetrahydrofuran: acetonitrile: 0.2% phosphoric acid solution: (14:7:79); column temperature: 45°C ; The flow rate is 1.0ml / min, the detection wavelength is 335nm; the number of theoretical plates is not ...

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Abstract

The invention provides a detection method of the content of wild baicalin in a traditional Chinese medicine, and belongs to the field of traditional Chinese medicines. The detection method comprises astep of preprocessing a sample and a step of injecting and detecting the sample, wherein the sample is herba erigerontis preferably; ethanol is adopted for extraction in preprocessing of the sample;the sample is injected in the conditions as follows: a C18-bonded packed column is adopted, a mobile phase comprises acetonitrile, tetrahydrofuran and 0.1%-0.2% phosphoric acid at a ratio of 7:14:79,the flow rate is 1.0 ml / min, and the column temperature is 40 DEG C. The detection method has the advantages of being stronger in adaptability, reducing the preprocessing step of the sample and more accurately reflecting the content of the wild baicalin in the traditional Chinese medicine.

Description

technical field [0001] The invention belongs to the technical field of quality control of Chinese medicinal materials, and in particular relates to a detection method of scutellarin in Chinese medicinal materials. Background technique [0002] Erigeron breviscapus (Erigeron breviscapus) is the dry whole plant of Erigeron breviscapus (Vant.) Hand-Mazz, a plant of the genus Asteraceae. The power of removing blood stasis, dredging collaterals and relieving pain is used for cold headache, rheumatism pain, paralysis caused by cerebrovascular accident, etc. ("National Chinese Herbal Medicine Compilation"). [0003] Scutellarin (breviscapus B) is an active ingredient of flavonoids isolated from Erigeron breviscapus (Vant.) Hand-Mazz. , breviscapine dripping pills, etc. Therefore, the content of scutellarin in breviscapine medicinal materials has become the symbolic component of Chinese medicinal materials used to determine the registration of breviscapine herb. [0004] The metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 林艳和李资磊唐琼杜江
Owner YUNNAN BIOVALLEY PHARMA CO LTD
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