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Method for simultaneously detecting multiple mycotoxins in milk

A mycotoxin and milk technology, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of low sensitivity, poor reliability, and weak stability, and achieve the effect of high sensitivity, strong stability, and good linear range

Inactive Publication Date: 2014-01-29
王加启 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As people pay more and more attention to mycotoxin contamination in milk, the UPLC-MS / MS simultaneous detection method of multiple mycotoxins in milk has become a research hotspot, but this method has defects such as low sensitivity, poor reliability, and weak stability to varying degrees. Room for improvement

Method used

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  • Method for simultaneously detecting multiple mycotoxins in milk
  • Method for simultaneously detecting multiple mycotoxins in milk
  • Method for simultaneously detecting multiple mycotoxins in milk

Examples

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Effect test

experiment example 1

[0042] Experimental Example 1 Mass Spectrometry Condition Optimization

[0043] Inject the standard solution through the syringe pump, positive and negative ion mode (ESI + and ESI-), select the ion with the highest relative ion abundance as the parent ion. Although OTA can be at ESI + In this study, ESI-mode was selected for detection, because it has higher sensitivity and stability in this mode. Due to the higher ionization efficiency in the corresponding modes, ZON and α-ZOL choose the negative ion mode, AFM 1 Select positive ion mode. In one injection test, the positive and negative ion modes are automatically switched by the positive and negative converter. The optimal precursor ions and ionization patterns for the four mycotoxins are shown in Table 3.

[0044] Table 3 Parent and daughter ions and mass spectrometry parameters

[0045]

[0046] Note: The ones marked with * are quantitative ions.

[0047] Note: Asterisk(*) indicates quantitative ion.

[0048] In ...

experiment example 2

[0049] Experimental Example 2 Selection of mycotoxin extractant

[0050] In this experiment, the extraction effect of mycotoxins from methanol and acetonitrile was compared, and the results showed that acetonitrile was used as the extraction solvent for four mycotoxins (aflatoxin M1, ochratoxin A, zearalenone and α-zearalenone). Alcohol) has a higher extraction efficiency ( figure 2 ).

[0051] The recovery rate R (%) is the ratio of the concentration of the spiked sample to the concentration of the standard solution, calculated according to the following formula:

[0052] R (%)=(Signal of spiked sample - signal of unspiked sample)×100 / signal of standard solution

experiment example 3

[0053] Experimental Example 3 Optimization of Purification Conditions of Mycotoxin Crude Extract

[0054] 1 Selection of purification column

[0055] Cleanup and enrichment steps have a dramatic effect on sensitivity in trace analysis. The results showed that when the unpurified and enriched mycotoxin crude extract samples were directly injected, there were many interference peaks and poor signals, and strong signal suppression occurred due to the matrix effect ( image 3 ), so direct injection of the mycotoxin extract cannot meet the detection requirements of the relevant limit standards, and it is necessary to purify and enrich the mycotoxin crude extract in the sample.

[0056] This experiment compares the Oasis HLB column (60mg, 3cm 3 ) and Mycosep226 column to purify and purify mycotoxin crude extract to select a more suitable purification column. The experimental results show that the purification and enrichment efficiency of the HLB column is relatively high, and the...

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Abstract

The invention discloses a method for simultaneously detecting multiple mycotoxins in milk. The method comprises the following steps: (1) extracting the mycotoxins from milk to obtain a crude mycotoxin extract; (2) purifying and concentrating the crude mycotoxin extract; (3) carrying out gradient eluting on the concentrated mycotoxins on a chromatographic column through a mobile phase and collecting eluate; and (4) qualitatively and quantitatively detecting the collected eluate by a mass spectrometer. An efficient, sensitive and stable method is created in the invention for simultaneously detecting aflatoxin M1, ochratoxin A, zearalenone and alpha-zearalenol in milk. The linearity, sensitivity, recovery, accuracy and reproducibility of the detection method disclosed by the invention are verified in fresh milk, liquid milk and milk powder, and as shown in the verification results, the detection method disclosed by the invention is good in linear range, high in sensitivity, good in credibility and strong in stability.

Description

technical field [0001] The invention relates to a method for detecting mycotoxins in milk, in particular to a method for simultaneously detecting aflatoxin M1, ochratoxin A, zearalenone and α-zearalen in milk by liquid chromatography tandem mass spectrometry The alcohol method belongs to the field of detection of mycotoxins in milk. Background technique [0002] Milk has become a necessity in people's lives, especially infant milk is the best substitute for breast milk, but mycotoxins have become one of the main quality and safety risk factors of milk, seriously threatening human health. In the process of milk processing, mycotoxins cannot be degraded by pasteurization or high-temperature sterilization, and mycotoxins can remain intact in milk products. Therefore, mycotoxins in milk have attracted more and more attention, especially yellow Aspergillus M 1 , ochratoxin A, zearalenone, and α-zearalenol are valued for their contamination levels and toxicity. [0003] At pres...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 王加启郑楠黄良策程建波李松励张养东
Owner 王加启
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