Method for detecting contents of citrinin in monascus by liquid chromatograph/mass spectrometer (LC/MS)

A liquid chromatography-mass spectrometry and citrinin technology, which is applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of long cycle and high testing cost, and achieve the effects of strong separation ability, accurate and reliable detection results, and high sensitivity.

Active Publication Date: 2011-09-07
CHENGUANG BIOTECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Enzyme-linked immunoassay is a relatively sensitive method at present, but this method requires special antibodies, which are not produced in China, and the test costs are expensive and the cycle is long

Method used

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  • Method for detecting contents of citrinin in monascus by liquid chromatograph/mass spectrometer (LC/MS)
  • Method for detecting contents of citrinin in monascus by liquid chromatograph/mass spectrometer (LC/MS)
  • Method for detecting contents of citrinin in monascus by liquid chromatograph/mass spectrometer (LC/MS)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. The experimental equipment and reagents are as follows

[0032] 1) Instrument: Waters liquid chromatography-mass spectrometry (American waters company); Chromatographic column: BEH C18 liquid chromatography column (50*2.1mm, 1.7μm) (American waters company); Syringe microporous membrane 0.22μm organic filter membrane; rotary evaporator (Shanghai Shenke); electronic balance (Mettler-Toledo Instrument Co., Ltd.); high-speed centrifuge (Xiangyi Group); ultrasonic instrument.

[0033] 2) Experimental reagents: standard citrinin, methanol, acetonitrile, formic acid, ultrapure water

[0034] Second, the experiment is as follows:

[0035] 1) In this embodiment, the citrinin standard substance was used to explore and determine the best chromatographic conditions and mass spectrometry conditions.

[0036] 2) Determining the sample to be tested by an established method to determine whether it contains citrinin.

[0037] 3) Add citrinin standard substance to the sample to be...

Embodiment 2

[0074] 1. The experimental equipment and reagents are as follows

[0075] 1) Instrument

[0076] Experimental apparatus is the same as embodiment one

[0077] 2) Experimental reagents

[0078] Experimental reagent is the same as embodiment one

[0079] 2. The experimental design is as follows:

[0080] 1) In this embodiment, the citrinin standard substance was used to explore and determine the best chromatographic conditions and mass spectrometry conditions.

[0081] 2) Determining the sample to be tested by an established method to determine whether it contains citrinin.

[0082] 3) Add citrinin standard substance to the sample to be tested, and determine the recovery rate, precision and minimum detection limit of the method.

[0083] 3. The test method is as follows:

[0084] 1) Extraction of citrinin in the sample

[0085] Accurately weigh 0.2 g of pigmented red yeast rice powder, put it in a 50 mL centrifuge tube; add methanol at a ratio of 1:10, and ultrasonically ...

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Abstract

The invention relates to a detection method of citrinin, in particular to a method for detecting contents of citrinin in monascus by liquid chromatograph / mass spectrometer (LC / MS). The method comprises the steps of pre-processing a sample by an ultrasonic extraction method, and performing ultrahigh-pressure liquid chromatograph and mass spectrometric detection. In the method, a waters BEH C18 liquid chromatographic column is adopted, the mobile phase is acetonitrile and water, and the gradient elution condition is that the column temperature is the room temperature; a quadrupole mass spectrometer detector is used: a spray source is electrosprayed in a positive ion manner, and parent ions and product ions are used as qualitative and quantitative ions; the result is that the linearity of the standard solution of citrinin in the method between 0.01 and 50 microgram / L is good; the regression equation is y=1923.2x+270.29, R2 is 0.9998; the recovery of the sample is 83.6%; the detection limit is 0.001 microgram / L. The accuracy of the method is high, the repeatability is good, and the method is suitable for the quantitative detection of citrinin in monascus.

Description

technical field [0001] The invention relates to a method for detecting citrinin, in particular to a method for detecting the content of citrinin in red yeast rice by using a liquid mass spectrometer. Background technique [0002] In our country, the use of Monascus to ferment and produce food and medicine has a history of thousands of years. Many traditional foods such as: red yeast rice, red yeast rice wine and fermented bean curd are deeply loved by people. Among the metabolites of Monascus, there are many valuable fermentation products in food, medicine and chemical industry. Such as natural monascus pigment with excellent quality, good coloring property and rich hue; Monacolin K which can significantly inhibit cholesterol synthesis and lower blood lipid levels; and very rich ergosterol, long-chain fatty acids and poly an antibacterial active substance. In the early 1990s, Europe, America, Japan and other countries saw a sharp increase in the demand for my country's edi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/72G01N30/34
Inventor 卢庆国王轩王磊刘东明唐建忠
Owner CHENGUANG BIOTECH GRP CO LTD
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