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A method for simultaneously preparing fumonisin b1, b2 and b3 standard substances

A technology of fumonisins and standard products, applied in the preparation of test samples, etc., can solve the problems of small amount of samples processed at one time, expensive scientific research, low recovery rate, etc., and achieve low preparation cost, strong repeatability, The effect of high purity standard

Active Publication Date: 2018-02-06
SHANGHAI ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high price of standard products makes it impossible for many scientific researches to continue
[0005] There are few literature reports on the separation and purification of fumonisins at home and abroad, mainly through silica gel chromatography column combined with thin layer chromatography and centrifugal partition chromatography for rough separation, but these methods have the disadvantages of small amount of samples processed at one time and high purity. Disadvantages such as low, low recovery and low preparation efficiency

Method used

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  • A method for simultaneously preparing fumonisin b1, b2 and b3 standard substances
  • A method for simultaneously preparing fumonisin b1, b2 and b3 standard substances
  • A method for simultaneously preparing fumonisin b1, b2 and b3 standard substances

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Embodiment 1

[0038] Example 1 Preparation of Fumonisins B1, B2, B3 Standards

[0039] 1. Sample extraction

[0040] The dried fumonisin-contaminated rice samples (random commercially available rice, screened out fumonisin-contaminated samples) were pulverized in a solid grinder and filtered through a 1 mm pore size mesh sieve. Take 200±0.01g of the sample powder and place it in a 2000mL jar, add 1000mL of acetonitrile-water (50:50, v / v) solution, place on a shaker at 150rpm and shake overnight, then filter with whatma5 filter paper. The filter cake was resuspended with 1000 mL of acetonitrile-water (50:50, v / v), shaken at 150 rpm for 2 h, and filtered. The two filtrates were combined and concentrated in a rotary evaporator at 40° C. until the content of acetonitrile in the extract was about 10% (v / v).

[0041] 2. Solid phase extraction column purification

[0042] Take 20mL of the extract and place it in a 50mL centrifuge tube, add 10mL of n-hexane, centrifuge at 3000r / min for 10min, di...

Embodiment 1

[0059] Carry out qualitative analysis and purity measurement to embodiment one preparation three kinds of standard products

[0060] 1 Qualitative analysis by liquid chromatography mass spectrometry (LC-MS / MS)

[0061] LC-MS / MS conditions: Thermo C18 chromatographic column (2.1mm×100mm, 5μm); mobile phase A is methanol, mobile phase B is aqueous solution containing 0.1% formic acid (v / v); gradient elution: 0~1mim, 50%B~50%B; 1-7min, 50%B~100%B; 7~8min, 100%B~100%B; 8~8.2min, 100%B~50%B; 8.2~9.0min, 50% B to 50% B; flow rate 300 μL / min; injection volume 5 μL; column temperature 30°C. Fragmentation voltage is 1.5V; spray voltage is 3.5kV; atomization air pressure adopts electrospray ESI ion source (both positive and negative ions are used), scanning force is 3500Pa; capillary temperature is 350°C; sheath air pressure is 45Pa; auxiliary air pressure is 15Pa. The scanning range is m / z300~800; the collision voltage of product ion fragments is 30eV.

[0062] Get FB 1 , FB 2 , F...

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Abstract

The invention provides a method for simultaneously preparing fumonisin B1, B2 and B3 standard products, the method comprising the following steps: sample extraction; rough purification; medium-pressure preparation. The method for simultaneously preparing fumonisins B1, B2 and B3 standard products of the present invention is stable and mature, and can be applied to the preparation of fumonisins in various grain matrices such as corn, rice, wheat, PDA, etc., with low cost and efficient preparation process Fast, high purity standard, good effect.

Description

technical field [0001] The invention relates to the technical field of agricultural product safety detection, in particular to a method for simultaneously preparing standard products of fumonisins B1, B2 and B3. Background technique [0002] Fumonisins are water-soluble secondary metabolites produced by Fusarium moniliforme under certain temperature and humidity conditions, the most important of which are fumonisins B1, B2 and B3, which can widely contaminate corn, wheat, rice Such crops have neurotoxicity, lung toxicity, liver toxicity, nephrotoxicity, carcinogenicity, and certain immunotoxicity, embryotoxicity and phytotoxicity, which have brought serious harm to human life, health and property safety of animals. [0003] Due to the strong toxicity and wide distribution of fumonisins, it has attracted great attention worldwide, and research on the detection technology of fumonisins B1, B2 and B3 has been carried out. Among them, the standard is an important carrier of mea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
Inventor 韩铮赵志辉郭文博沈源源
Owner SHANGHAI ACAD OF AGRI SCI
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