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A kind of detection method of citrinin in Zhibitu tablets

A detection method, the technology of Zhibituo Tablets, is applied in the field of chemical detection to achieve high-sensitivity analysis and reduce the use of toxic reagents

Active Publication Date: 2017-07-11
WUZHOU INST FOR FOOD & DRUG CONTROL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In China, the Chinese Pharmacopoeia has not yet used citrinin as a control indicator for Chinese patent medicines containing red yeast rice

Method used

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  • A kind of detection method of citrinin in Zhibitu tablets
  • A kind of detection method of citrinin in Zhibitu tablets
  • A kind of detection method of citrinin in Zhibitu tablets

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Embodiment 1

[0018] 1 material

[0019] 1.1 Instrument

[0020] Agilent1295-6550C triple quadrupole liquid chromatography-mass spectrometer (Agilent, USA), HLB-SPE column (60mg / 3ml, Shanghai Anpu Scientific Instrument Co., Ltd.), Agilent ZORBAX Eclipse Plus (2.1×50mm, 1.8μm; Agilent, USA ), XA205DU electronic balance (Mettler Toledo, Germany), ultrasonic cleaner.

[0021] 1.2 Zhibituo tablets and reagents

[0022] Three batches of Zhibituo Tablets were obtained from market samples.

[0023] Citrinin (batch number: 518-75-2-150403, standard product purchased from Pribolab, purity > 98%), ethanol and methanol are chromatographically pure, other reagents are analytically pure, experimental water is purified by ELGA PURELAB ClassicUVF system Filtered deionized water.

[0024] The percentage concentration involved in the present invention, unless otherwise specified, refers to the volume concentration of the liquid, and refers to the mass concentration when the solute is a solid.

[0025] ...

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PUM

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Abstract

The invention provides a method for detecting citrinin in Zhibituo tablets, aiming to provide a method for detecting citrinin in Zhibituo tablets with high sensitivity and short detection time; the method comprises the following steps in turn: 1) Preparation of standard solution; 1) Preparation of standard solution; 2) Take 0.5g of Zhibituo tablets and pulverize them, put them in a 10ml Erlenmeyer flask, add 3ml of 1% phosphoric acid-methanol solution, heat and reflux at 60°C for 60min, cool, filter, Transfer the filtrate to a 25ml volumetric flask, dilute to the mark with water, shake well and filter, pass through the HLB solid-phase extraction column activated with 3ml ethanol and 3ml water respectively at a flow rate of 1ml / min, rinse with 5ml water, discard, and then Elute with 5ml of ethanol to collect the eluate, blow the eluate to nearly dry under nitrogen at 40°C, add 1ml of ethanol to dissolve it, and filter it with a 0.22μm organic filter membrane to obtain the sample to be tested. The invention relates to detection by a triple quadrupole liquid phase mass spectrometer; it belongs to the technical field of chemical detection.

Description

technical field [0001] The invention provides a method for detecting citrinin, specifically a method for detecting citrinin in Zhibituo tablets; it belongs to the technical field of chemical detection. Background technique [0002] Citrinin was first isolated from Penicillium citrinum in 1931. Its molecular formula is C 13 h 14 o 5 , the molecular weight is 250.25. Citrinin has certain nephrotoxicity and hepatotoxicity, can cause teratogenicity, cause tumor and induce mutation. Red yeast rice is a traditional Chinese medicinal material, which is cultivated and fermented in rice with a unique monascus mold. Because some Monascus strains can produce statins that inhibit cholesterol biosynthesis, the traditional Chinese medicine Monascus has been developed as Zhibituo Tablets and health food for lowering blood lipids. In 1995, after the French scholar Blanc et al. first discovered that citrinin was contained in red yeast rice products, citrinin has been used as a strict c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 陈学松罗达龙王华
Owner WUZHOU INST FOR FOOD & DRUG CONTROL
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