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Method for detecting citrinin in monascus pigment powder by solid-phase extraction-liquid chromatography mass spectrometry

A technology of monascus pigment and citrinin, which is applied in the detection field of solid phase extraction-liquid mass tandem detection of citrinin and citrinin in monascus pigment powder

Inactive Publication Date: 2016-08-31
WUZHOU INST FOR FOOD & DRUG CONTROL
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  • Abstract
  • Description
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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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  • Method for detecting citrinin in monascus pigment powder by solid-phase extraction-liquid chromatography mass spectrometry
  • Method for detecting citrinin in monascus pigment powder by solid-phase extraction-liquid chromatography mass spectrometry
  • Method for detecting citrinin in monascus pigment powder by solid-phase extraction-liquid chromatography mass spectrometry

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Experimental program
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Effect test

Embodiment 1

[0022] 1 material

[0023] 1.1 Instrument

[0024] Agilent1290-6490 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.

[0025] 1.2 Monascus pigment powder and reagents

[0026] Two batches of red yeast rice pigment powder were obtained from market samples.

[0027] Citrinin (batch number: 518-75-2-150403, the standard product was purchased from Pribolab, purity > 98%), methanol and acetonitrile were chromatographically pure, other reagents were analytically pure, and the experimental water was purified by the ELGA PURELAB ClassicUVF purification system Filtered deionized water.

[0028] The percentage concentration involved in the present invention, unless otherwise specified, refers to the volume concentration of the liquid, and refers to the...

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Abstract

The invention provides a method for detecting citrinin in monascus pigment powder by solid-phase extraction-liquid chromatography mass spectrometry and aims to provide a method for detecting citrinin in monascus pigment powder by solid-phase extraction-liquid chromatography mass spectrometry with high sensitivity and accurate qualitative and quantitative detection. The method successively comprises the following steps: 1) preparation of a standard solution; 2) sample pretreatment; and 3) sample purification. The method comprises the following steps: letting a sample pretreatment solution pass through an HLB solid-phase extraction column at the flow rate of 1ml / min; leaching with 5 ml of water, discarding, eluting with 5 ml of methanol and collecting an eluant, nitrogen-blowing the eluant at 40 DEG C to dry, precisely adding 1 ml of a methanol for dissolution, filtering with 0.22 microns of an organic filter membrane, and detecting by loading a sample to be measured onto a chromatographic column. The invention 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 monascus pigment powder by solid-phase extraction-liquid mass tandem; 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 a blood lipid-lowering Monascus pigment powder and health food. In 1995, after the French scholar Blanc et al. first discovered that citrinin was contained in red y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 陈学松罗达龙王华
Owner WUZHOU INST FOR FOOD & DRUG CONTROL
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