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Method for detecting seven typical mycotoxins in fruits and vegetables simultaneously

A mycotoxin, a typical technology, applied in the field of simultaneous detection of 7 typical mycotoxins in fruits and vegetables, can solve the problem of few and single mycotoxins, and achieve high-efficiency extraction, low detection limit, simple and reliable results

Active Publication Date: 2018-08-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, there are few reports on the detection of mycotoxins in fresh fruits and vegetables, and most of the reported researches on the detection of mycotoxins in fruits and vegetables focus on the detection of a single target or several mycotoxins of the same species.

Method used

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  • Method for detecting seven typical mycotoxins in fruits and vegetables simultaneously
  • Method for detecting seven typical mycotoxins in fruits and vegetables simultaneously
  • Method for detecting seven typical mycotoxins in fruits and vegetables simultaneously

Examples

Experimental program
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Effect test

Embodiment 1

[0041]The establishment of mass spectrometry conditions in this embodiment:

[0042] Among the 7 target substances, TEN contains amino groups, and the [M+H] with a higher response is obtained in the positive mode of ESI + peak; OTA contains a phenylalanine group, which responds in both positive and negative ESI modes, but in the positive mode, the abundance of molecular ion peaks is higher and the signal is more stable, so the positive mode is selected for detection; the remaining 5 compounds Both obtained higher abundance [M-H] in ESI negative mode - peak. According to 2002 / 657 / EC, two main characteristic fragment ions were selected as the qualitative and quantitative ions for each compound, and the intensity of the characteristic fragment ions was maximized by optimizing parameters such as collision voltage. The optimized mass spectrometry conditions are shown in Table 1. Combining the chromatographic conditions finally determined by the present invention and the chromatog...

Embodiment 2

[0048] The establishment of the present embodiment chromatographic conditions:

[0049] In the experiment, a BEH C18 (100mm×2.1mm, 1.7μm) chromatographic column was used as a separation column to compare acetonitrile-water, acetonitrile-0.1% formic acid water, acetonitrile-0.05% ammonia water, acetonitrile-10mmol / L ammonium acetate, acetonitrile-10mmol / The effect of L ammonium bicarbonate group 5 mobile phase system on the target response and separation effect. The results showed that the peak shape and overall response of the seven compounds to be tested were the best in the ammonium acetate system; no chromatographic peaks were seen in the ammonium bicarbonate system for PAT; Severely inhibited, the peak shape of TeA in water, ammonia water and formic acid water system has serious tailing, and PAT and DON are unstable under alkaline conditions. Therefore, the present invention finally selects the acetonitrile-10mmol / L ammonium acetate mobile phase system.

[0050] Further...

Embodiment 3

[0053] Optimization of extraction conditions in this embodiment:

[0054] PAT is easily soluble in water and organic solvents such as ethyl acetate, acetone and ethanol; OTA and DON are soluble in polar organic solvents such as methanol, ethanol, acetonitrile and ethyl acetate; AOH, AME, TeA and TEN are also soluble in large Some organic solvents; TeA (pKa=3.5) and OTA (pKa=4.4) are acidic, and when the pH value of the extraction system is lower than the pKa value, it is beneficial to promote the distribution of these two analytes in the organic phase. According to the above properties and the principle of "like dissolves like", and minimize the extraction of other matrix components, the experiment compared 1% formic acid-acetonitrile (FA-ACN, volume ratio), 0.1mol / L HCl-acetonitrile (HCl- ACN), 1% formic acid-ethyl acetate (FA-EAC, volume ratio), 0.1mol / L HCl-ethyl acetate (HCl-EAC) extraction effect of four extraction systems.

[0055] The negative lettuce samples were sele...

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Abstract

The invention belongs to the technical field of food detection, and discloses a method for detecting seven typical mycotoxins in fruits and vegetables simultaneously. The method includes subjecting to-be-detected fruit and vegetable samples to ultrasonic extraction by formic acid-acetonitrile, performing centrifugation, drying supernatant, adding a formic acid aqueous solution before evenly mixing, performing extraction by an HLB (hydrophile-lipophile balance) solid-phase extraction column, and redissolving extract in a mixed solution of a ammonium acetate aqueous solution and acetonitrile toobtain to-be-tested liquid; preparing a mixed standard solution containing the seven typical mycotoxins, namely AOH, AME, TeA, TEN, DON, PAT and OTA, from the mixed solution of the ammonium acetate aqueous solution and the acetonitrile, acquiring a standard curve through UHPLC-MS / MS detection, detecting the to-be-detected liquid under same conditions, and calculating the contents of the seven typical mycotoxins in the to-be-tested liquid according to the standard curve. The method is applicable to simultaneous determination of four major types of the seven mycotoxins in the fruits and the vegetables, makes up for the defect of singularity of detection targets, and has the advantages of low detection limit and high detection accuracy.

Description

technical field [0001] The invention belongs to the technical field of food detection, and in particular relates to a method for simultaneously detecting seven typical mycotoxins in fruits and vegetables. Background technique [0002] Fruits and vegetables have high water content and rich nutrition. During the process of growth, harvesting, storage and transportation, they are extremely vulnerable to infection by various pathogenic bacteria and rot, producing and accumulating various mycotoxins. Most mycotoxins are stable in nature, and it is difficult to completely remove them under conventional storage, transportation and processing conditions, which will pose a potential threat to human and animal health. Studies have shown that the mycotoxins that contaminate fruits and vegetables mainly include alternaria toxins, ochratoxin A (OTA), patulin (PAT) and trichothecenes. Alternaria toxins are a series of metabolites produced by Alternaria, which are phytopathogenic bacteria...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 肖凯军董浩王震朱良王兆梅
Owner SOUTH CHINA UNIV OF TECH
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