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Detection method of citrinin in Xuezhikang capsules

A technology of Xuezhikang capsule and citrinin is applied in the field of chemical detection to achieve the effect of reducing the use of toxic reagents and high-sensitivity analysis

Inactive Publication Date: 2016-08-31
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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  • Detection method of citrinin in Xuezhikang capsules
  • Detection method of citrinin in Xuezhikang capsules
  • Detection method of citrinin in Xuezhikang capsules

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Experimental program
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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 Guoxuezhikang Capsules and Reagents

[0022] The 4 batches of Guoxuezhikang Capsules are all from market samples. 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.

[0023] 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.

[0024] 2 M...

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Abstract

The invention provides a detection method of citrinin in Xuezhikang capsules and aims to provide a method for detecting citrinin in Xuezhikang capsules with high sensitivity and short detection time. The method successively comprises the following steps: 1) preparing a standard solution; 2) fetching 0.5 g of contents from capsules, placing the contents into a 10ml conical flask, adding 3ml of 1% acetic acid-methanol solution, carrying out ultrasonic extraction for 30 min, cooling, filtering, transferring a filtrate into a 25ml volumetric flask, adding water to a constant volume, shaking up and filtering, loading through a C18 solid-phase extraction column at the flow velocity of 1ml / min, leaching with 5 ml of water, discarding, eluting with 5 ml of ethanol and collecting an eluant, nitrogen-blowing the eluant at 40 DEG C to dry, precisely adding 1ml of ethanol and dissolving, filtering with 0.22 micron organic filter membrane so as to obtain a sample to be detected, and detecting the sample to be detected through an Agilent1295-6550C triple quadrupole liquid chromatograph-mass spectrometer. The invention belongs to the field of chemical detection technology.

Description

technical field [0001] The invention provides a method for detecting citrinin, specifically a method for detecting citrinin in Xuezhikang capsules, belonging 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 Guoxuezhikang Capsules 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 ...

Claims

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Application Information

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