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LC-Q-TOF/MS detection technology for 544 pesticide residues in stone fruits

A Q-TOF, pesticide residue technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of high price, loopholes in food safety monitoring, and only 2 or 3 years of validity, and achieve the effect of large amount of information

Inactive Publication Date: 2016-06-15
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 technology for 544 pesticide residues in stone fruits
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in stone fruits
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in stone fruits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in stone fruit (taking peach as an example), including the following steps:

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

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

[0069] 1.2 Weigh 10g of peach sample (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 magnesium sulfate , shake for 5 min, centrifuge at 4200 r / min for 5 min, take 20 mL of the supernatant, concentrate it to about 1 mL by rotary evaporation in a 40°C water bath, 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 + toluene (3+1, v / v) first, and discard th...

Embodiment 2

[0099] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in stone fruit (taking apricot 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 Figure 6 .

[0102] LC-Q-TOF / MS detection results in apricot samples in a certain area: 7 commercial pear samples were collected in a certain area, and 544 kinds of pesticide residues were detected by LC-Q-...

Embodiment 3

[0106] Implementation examples of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in stone fruit (jujube as an example) samples.

[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 jujube samples in a certain area: 9 commercially available jujube samples in a certain area were collected, and 544 kinds of pesticide residues were det...

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Abstract

The invention provides an LC-Q-TOF / MS detection technology for 544 pesticide residues in stone fruits. The technology includes the steps of: 1) under a TOF / MS mode in the LC-Q-TOF / MS, respectively measuring retention time of each pesticide reference substance under the certain chromatography-mass spectrometry conditions; 2) determining the ionization formation and chemical formula of the compound with an ESI source to obtain accurate mass number of a parent ion of each compound to form a TOF / MS database; 3) under a Q-TOF / MS mode, respectively collecting fragment ion mass spectrograms under 3-5 different collision energy of each pesticide reference substance, and introducing the collected information to PCDL software to obtain a Q-TOF / MS database; 4) comparing the retention time, primary mass spectrum and secondary mass spectrum of the sample of the stone fruits to determine whether the pesticide residues exist in the sample or not, and meanwhile, performing secondary determination to the compound having higher primary score, and if secondary score is high, determining existence of the pesticide residues. The technology is quick, high-throughput, high-precision and high-reliability, and can be used for accurately screening the pesticides in the stone fruits.

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 drupe fruits. 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 of more a...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72G01N2030/027
Inventor 庞国芳范春林彭兴常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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