LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables

A Q-TOF, pesticide residue technology, applied in the fields of food hygiene and agricultural product safety testing, can solve the problems of high price, loopholes in food safety monitoring, and the validity period is only 2 or 3 years, and achieves the effect of large amount of information

Inactive Publication Date: 2016-07-20
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the actual work of pesticide and veterinary drug residue laboratories, most laboratories do not store hundreds of pesticide standard products. The reason is that pesticide standard products are not only expensive, but also valid for only 2 or 3 years, requiring repeated investment.
There are only dozens of standard pesticides in general laboratories, and the types of pesticides that are routinely monitored are limited to these dozens, resulting in loopholes in food safety monitoring

Method used

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  • LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables
  • LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables
  • LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] An implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in solanaceous vegetables (taking sweet pepper as an example), including the following steps:

[0067] 1. Specific steps of sample pretreatment technology:

[0068] 1.1 Take the edible part of the sweet pepper sample, chop it up, mix it evenly, seal it, and mark it;

[0069] 1.2 Weigh 10g of sweet pepper samples (accurate to 0.01g), add 40mL of 1% acetic acid acetonitrile into an 80mL centrifuge tube, use a high-speed homogenizer at 13500r / min, homogenize and extract for 1min, add 1g of sodium chloride, 4g of anhydrous sulfuric acid Magnesium, shake for 5min, centrifuge at 4200r / min for 5min, take 20mL of the supernatant, concentrate it to about 1mL by rotary evaporation in a water bath at 40°C, and wait for purification.

[0070] 1.3 in Carbon / NH 2 Add about 2cm high anhydrous sodium sulfate to the column. Rinse the SPE column with 4 mL of acetonitrile + t...

Embodiment 2

[0099] Implementation examples of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in solanaceous vegetables (taking tomato as an example).

[0100] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.

[0101] Measure the sample solution in full-scan mode, compare the detection results with the TOF database, and obtain the first-level TOF score, see Figure 4 ; For compounds whose scores meet the requirements, establish a secondary acquisition method in the software, see Figure 5 ;In MS / MS mode, re-run the sample solution to obtain the full scan data of the sample fragment ions, compare it with the fragment ion information in the MS / MS library, and obtain the secondary QTOF score, see Image 6 .

[0102] LC-Q-TOF / MS detection results in tomato samples in a provincial capital city: 12 tomato samples sold in a provincial capital city were collected, and 544 kinds of pesticide res...

Embodiment 3

[0106] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in solanaceous vegetables (eggplant as an example).

[0107] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.

[0108] Measure the sample solution in full-scan mode, compare the detection results with the TOF database, and obtain the first-level TOF score, see Figure 7 ; For compounds whose scores meet the requirements, establish a secondary acquisition method in the software, see Figure 8 ;In MS / MS mode, re-run the sample solution to obtain the full scan data of the sample fragment ions, compare it with the fragment ion information in the MS / MS library, and obtain the secondary QTOF score, see Figure 9 .

[0109] LC-Q-TOF / MS detection results in eggplant samples in a provincial capital city: 18 commercially available eggplant samples in a provincial capital city were collected, and 544 kinds...

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Abstract

The invention provides an LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables. In a TOF/MS mode, LC-Q-TOF/MS measures the retention time of each pesticide standard substance under specified chromatographic and mass spectrometric conditions, an ionization form and a chemical formula of each compound under an ESI source are determined, the exact mass number for parent ions of each compound is obtained, and a TOF/MS database is formed. In a Q-TOF/MS mode, fragment ion mass spectra of each pesticide standard substance in 3-5 different collision energies are collected respectively, the collected information is introduced into PCDL software, and a Q-TOF/MS database is formed. Through comparison of the retention time and first-level mass spectrometry and second-level mass spectrometry information of solanaceous fruit vegetable samples, whether the samples contain the pesticide residues is determined, compounds having higher first-level score are subjected to second-level confirmation, and if the second-level score is higher, related pesticide residues are confirmed to be detected out. The method has the advantages of high speed, high throughput, high precision, high reliability and the like, and can accurately screen the pesticides in the solanaceous fruit vegetables.

Description

technical field [0001] The invention relates to the fields of food hygiene and agricultural product safety detection, in particular to a method for detecting 544 kinds of pesticide residues in solanaceous vegetables. Background technique [0002] As early as 1976, the World Health Organization (WHO), the Food and Agriculture Organization (FAO) and the United Nations Environment Program (UNEP) jointly established the Global Environment Monitoring System / Food Project (Global Environment Monitoring System, GEMS / Food), aiming to grasp the status of food contamination in member countries , understand the intake of food pollutants, protect human health, and promote trade development. Now, all countries in the world have raised food safety to the strategic position of national security. Pesticide residue limit is one of the food safety standards and also the entry threshold for international trade. At the same time, the requirements for pesticide residues show a development trend...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 庞国芳范春林康健常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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