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LC-Q-TOF/MS detection technology for 544 pesticide residues in kernel fruit

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: 2016-08-03
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 kernel fruit
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in kernel fruit
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in kernel fruit

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 pome fruits (taking apples as an example), including the following steps:

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

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

[0069] 1.2 Weigh 10g of apple 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 the e...

Embodiment 2

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

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

[0101] Detection of Pesticide Residues in Pome Fruits (Take Pear as an Example) Samples

[0102] 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 .

[0103] LC-Q-TOF / MS detection results in pear samples from a certain area: 19 commercial pear samples were...

Embodiment 3

[0107] An implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in pome fruits (take hawthorn as an example) includes the following steps:

[0108] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.

[0109] Detection of pesticide residues in pome fruits (take hawthorn as an example) samples

[0110] 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 .

[0111] LC-Q-TOF / MS detection results in hawthorn samples from a cer...

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Abstract

The invention provides an LC-Q-TOF / MS detection technology for 544 pesticide residues in kernel fruit. In a TOF / MS mode, the LC-Q-TOF / MS detection technology separately determines the retention time of each pesticide standard under designated gas chromatography-mass spectrography conditions, determines the ionization form and chemical formula of a compound under the condition of an ESI source and acquires the accurate mass number of the parent ion of each compound so as to form a TOF / MS database. In a Q-TOF / MS mode, the LC-Q-TOF / MS detection technology separately acquires the fragment ion mass spectrum of each pesticide standard under the condition of three to five different collision energies and introduces acquired information into PCDL software so as to form a Q-TOF / MS database. Through comparison of the retention time, mass spectrometry information and tandem mass spectrometry information of a kernel fruit sample, whether the sample contains pesticide residues or not can be determined; and compounds with high primary scores are subjected to secondary confirmation, and if secondary scores are high, it is confirmed that related pesticide residues are detected. The LC-Q-TOF / MS detection technology provided by the invention has the advantages of fastness, high throughput, high accuracy, high reliability and the like, and can accurately screen pesticides in the kernel fruit.

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 pome 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 an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 庞国芳范春林曹亚飞常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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