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Extracting, purification and detection method for nivalenol in grains
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A technology for fusarium nivalenol and a detection method, which is applied in the field of analysis and testing, can solve the problems of matrix interference and high cost of purification methods, and achieves the effects of low cost, omitting derivatization operation steps, and reducing usage.
Active Publication Date: 2013-10-16
JIANGSU ACAD OF AGRI SCI
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[0006] The purpose of the present invention is to solve the actual problem that there are many impurity peaks in the detection of ultraviolet detectors, which are seriously interfered by the matrix, and the cost of the purification method is high. , providing a method suitable for the extraction, purification and detection of nivalenol
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Embodiment 1
[0017] 1. Selection of standard samples:
[0018] Standard samples were purchased from Sigma-Aldrich Company (the same below).
[0019] 2. Extraction and purification method of nivalenol in wheat:
[0020] (1) Sample preparation: Weigh 5.0 g of the crushed wheat sample into a 50 ml centrifuge tube, add 25 ml of H 2 O shake and extract for 20min, centrifuge the extract at 3000rpm for 10min, discard the precipitate, take 10ml of the supernatant and add an equal volume of absolute ethanol to precipitate at 4°C for 1h, centrifuge at 10000rpm for 15min, discard the precipitate, take the supernatant at 50°C Rotary evaporated to dryness, 1.0ml H 2 O was extracted by shaking twice, combined with 2.0ml of the extract, and further purified by a Waters OASIS HLB solid-phase extraction column with a specification of 3ml / 60mg:
[0021] (2) The steps to use the OASIS solid-phase extraction cartridge are as follows:
[0022] a. Activation of small column: After rinsing with 2ml methanol,...
Embodiment 2
[0029] 1. Extraction and purification method of nivalenol in corn:
[0030] (1) Sample preparation: Weigh 5.0 g of crushed corn sample into a 50 ml centrifuge tube, add 25 ml of H 2 O shake and extract for 20min, centrifuge the extract at 3000rpm for 10min, discard the precipitate, take 10ml of the supernatant and add an equal volume of absolute ethanol to precipitate at 4°C for 1h, centrifuge at 10000rpm for 15min, discard the precipitate, take the supernatant at 50°C Rotary evaporated to dryness, 1.0ml H 2 O was extracted by shaking twice, combined with 2.0ml of the extract, and further purified by a Waters OASIS HLB solid-phase extraction column with a specification of 3ml / 60mg:
[0031] (2) The steps to use the OASIS solid-phase extraction cartridge are as follows:
[0032] a. Activation of small column: After rinsing with 2ml methanol, add 2ml H 2 O rinse at natural flow rate, and then vacuum dry; b. Loading: sample volume is 2.0ml, natural flow rate, and then use 3.0m...
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Abstract
The invention provides an extracting, purification and detection method for nivalenol in grains, which adopts water for extracting samples and leads extracting liquid to be deposited by ethanol and combined with a solid phase extraction method so as to remove interference of impurities. The purified samples are performed with qualitative and quantitative analysis on a high performance liquid chromatography-ultraviolet detector. The extracting, purification and detection method is high in accuracy, good in repeatability, small in blend peak interference and low in cost, requires no frequent replacing of a protection column, greatly reduces using of organic solvent, and is suitable for mass detection of the nivalenol in grains.
Description
technical field [0001] The invention relates to an extraction, purification and detection method for nivalenol in cereals, and belongs to the field of analysis and testing. Background technique [0002] Head blight caused by Fusarium is one of the most important diseases of cereal crops, seriously affecting the world's food security. Fusarium toxins are a class of secondary metabolites produced by Fusarium fungi. Trichothecenes contain more than 200 compounds and are a very important class of Fusarium toxins. Deoxynivalenol (DON), Nivalenol (NIV) and their derivatives belong to trichothecene family B, the basic structure is a tetracyclic sesquiterpene, with C8 The carbonyl at the position is characteristic. Among them, DON ranks first in the contamination rate and level of grain contamination by Fusarium toxins, posing a huge threat to the health of humans and livestock. Studies in recent years have shown that NIV may be related to human esophageal cancer, IgA nephropath...
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