LC-Q-TOF/MS detection technology for 544 pesticide residues in melon vegetables

A Q-TOF technology for melons and vegetables, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of high price, loopholes in food safety monitoring, valid period of only 2 or 3 years, etc., 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 melon vegetables
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in melon vegetables
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in melon 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 melon vegetables (taking cucumber as an example), including the following steps:

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

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

[0069] 1.2 Weigh 10g of cucumber 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 2em high anhydrous sodium sulfate to the column. Rinse the SPE column with 4mL acetonitrile + toluene (3+1, v / v) first, a...

Embodiment 2

[0100] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in melon vegetables (take zucchini as an example).

[0101] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.

[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 of zucchini samples in a provincial capital city: 16 commercially available zucchini samples were collected in a provincial capital city, and 544 kinds o...

Embodiment 3

[0107] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in melon vegetables (take bitter gourd as an example).

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

[0109] 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 .

[0110] LC-Q-TOF / MS detection results of bitter gourd samples in a provincial capital city: 7 commercially available bitter gourd samples were collected in a provincial capital city, and...

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Abstract

The present invention establishes a LC-Q-TOF/MS detection technology for 544 kinds of pesticide residues in melon vegetables. LC-Q-TOF/MS in TOF/MS mode, respectively measure the retention time of each pesticide standard under the specified chromatographic mass spectrometry conditions, determine the ionization form and chemical formula of the compound under the ESI source, and obtain the parent ion of each compound Accurate mass number of the TOF/MS database. In the Q-TOF/MS mode, the fragment ion mass spectra of each pesticide standard were collected under 3-5 different collision energies, and the collected information was imported into the PCDL software to form a Q-TOF/MS database. By comparing the retention time, primary mass spectrometry and secondary mass spectrometry information in melon and vegetable samples, determine whether the sample contains pesticide residues, and perform secondary confirmation on compounds with higher primary scores. If the secondary score is higher, it is confirmed Relevant pesticide residues were detected. The invention has the advantages of rapidity, high throughput, high precision, high reliability and the like, and can accurately screen pesticides in melons and 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 melon 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 of mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89G01N30/06
CPCG01N30/89G01N30/06
Inventor 庞国芳范春林康健常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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