UPLC-PDA (Ultra Performance Liquid Chromatography-Photodiode array) and QAMS (Quantitative Amplification Mass Spectrometry) combined detection method for Wujin granules

A detection method and particle technology, which is applied in the detection field of UPLC-PDA combined with QAMS, can solve the problems of spot interference, various reagents, and great harm to human body and environment, and achieve high accuracy and reproducibility

Active Publication Date: 2020-06-23
山东省兽药质量检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0020] The identification results using this method are stable, obvious, and reproducible, but there are many reagents used for TLC identification, such as cyclohexane, isopropanol, petroleum ether, ethyl acetate, etc., which are harmful to human body and environment and pollute greatly. substances, and the spots are easily disturbed by various external factors such as relative humidity and temperature
When performing qualitative and quantitative determination of the main components, it is necessary to prepare two different mobile phases and use different chromatographic conditions for detection, which is time-consuming and laborious. It takes at least two or three days for the detection of a sample

Method used

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  • UPLC-PDA (Ultra Performance Liquid Chromatography-Photodiode array) and QAMS (Quantitative Amplification Mass Spectrometry) combined detection method for Wujin granules
  • UPLC-PDA (Ultra Performance Liquid Chromatography-Photodiode array) and QAMS (Quantitative Amplification Mass Spectrometry) combined detection method for Wujin granules
  • UPLC-PDA (Ultra Performance Liquid Chromatography-Photodiode array) and QAMS (Quantitative Amplification Mass Spectrometry) combined detection method for Wujin granules

Examples

Experimental program
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Effect test

Embodiment 1

[0053] A detection method for Wujin particles, comprising the following steps:

[0054] (1) take by weighing berberine hydrochloride, palmatine hydrochloride, honokiol, magnolol reference substance respectively, and dilute with methanol respectively and constant volume, obtain the stock solution of four kinds of medicines;

[0055] specific:

[0056] Berberine hydrochloride reference substance, content 86.7%, provided by China National Institutes for Food and Drug Control, accurately weighed 30.09mg, diluted with methanol and adjusted to 100mL;

[0057] Palmatine hydrochloride reference substance, content 86.2%, provided by China National Institutes for Food and Drug Control, accurately weighed 10.38mg, diluted with methanol and adjusted to 100mL;

[0058] Honokiol reference substance, content 98.4%, provided by China National Institute for the Control of Pharmaceutical and Biological Products, accurately weighed 12.52mg, diluted with methanol and adjusted to 100mL;

[0059]...

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Abstract

The invention belongs to the technical field of veterinary drug detection, and particularly relates to a UPLC-PDA and QAMS combined detection method for Wujin granules. According to the detection method, an ultra-high performance liquid chromatography-photodiode array detection method is adopted, a spectrogram is used for identification, and a chromatogram is used for quantitative content detection. A quantitative analysis of multiple components by single marker is established, honokiol is used as an internal reference substance, relative correction factors between honokiol and palmatine hydrochloride, berberine hydrochloride and magnolol are established, and content calculation is carried out by using the obtained relative correction factors, so that quantitative analysis of multiple components by single marker is realized. According to the method, the four substances can be quickly qualitatively and quantitatively detected, the method is high in accuracy and reproducibility, purchaseand investment of reference substances are reduced, and funds are saved.

Description

technical field [0001] The invention belongs to the technical field of veterinary drug detection, and in particular relates to a detection method of UPLC-PDA combined with QAMS for Wujin granules. Background technique [0002] The Ministry of Agriculture of the People's Republic of China announced No. 164 in 2019, promulgating that Wujin Granules has obtained a new veterinary drug certificate and promulgating its testing quality standards. Wujin Granules 【Function】 astringent intestines, antidiarrheal, clearing away heat and dampness. [Indications] Lamb dysentery. [0003] The standards are as follows: [0004] [Identification] (1) Take 5g of this product, grind it finely, add 30ml of methanol, heat and reflux for 30 minutes, let it cool, filter, evaporate to dryness, add 20ml of water to the residue to dissolve, extract 3 times with ether, 20ml each time, combine ether solution, evaporated to dryness, and the residue was dissolved in 1ml of methanol as the test solution....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/04G01N30/74G01N30/86G01N30/12G01N30/88
CPCG01N30/02G01N30/06G01N30/14G01N30/04G01N30/74G01N30/8634G01N30/12G01N30/8679G01N30/88G01N2030/126G01N2030/146G01N2030/045G01N2030/884
Inventor 魏秀丽张传津张志民李有志杨林杨志昆冯涛
Owner 山东省兽药质量检验所
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