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LC-Q-TOF/MS (liquid chromatography-quadrupole-time of flight/mass spectrometry) technology for detecting 544 kinds of pesticide residues in melons and fruit

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: 2016-04-13
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 (liquid chromatography-quadrupole-time of flight/mass spectrometry) technology for detecting 544 kinds of pesticide residues in melons and fruit
  • LC-Q-TOF/MS (liquid chromatography-quadrupole-time of flight/mass spectrometry) technology for detecting 544 kinds of pesticide residues in melons and fruit
  • LC-Q-TOF/MS (liquid chromatography-quadrupole-time of flight/mass spectrometry) technology for detecting 544 kinds of pesticide residues in melons and 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 melons and fruits (taking watermelon as an example), including the following steps:

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

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

[0069] 1.2 Weigh 10g of watermelon 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, extract the homogenate 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 / ...

Embodiment 2

[0100] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in melons and fruits (take Hami melon 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 in cantaloupe samples in a provincial capital city: 5 commercially available cantaloupe samples in a provincial capital city were collected, and 544 k...

Embodiment 3

[0107] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in melons and fruits (taking melon 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 in melon samples in a provincial capital city: 9 commercially available melon samples in a provincial capital city were collected, and 544 kinds of pest...

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Abstract

The invention provides LC-Q-TOF / MS (liquid chromatography-quadrupole-time of flight / mass spectrometry) technology for detecting 544 kinds of pesticide residues in melons and fruit. In a TOF / MS mode, LC-Q-TOF / MS is used for respectively determining the retention time of each pesticide standard substance under specified chromatography-mass spectrometry conditions, determining the ionization forms and chemical formula of the compound under the condition of ESI (electron spray ionization) and obtaining the precise mass number of the parent ion of each compound, thus forming a TOF / MS database. In a Q-TOF / MS mode, the fragment ion mass spectrum of each pesticide standard substance under 3-5 different collision energy is respectively collected and the collected information is imported into PCDL software, thus forming a Q-TOF / MS database. Whether samples contain pesticide residues is determined by comparing the retention time and primary and secondary mass spectrometry information of melon and fruit samples, secondary confirmation is carried out on the compounds with higher primary scores, and detection of related pesticide residues is confirmed if the secondary scores are higher. The technology has the advantages of rapidness, high throughput, high precision, high reliability, and the like and can be used for precisely screening pesticides in the melons and 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 melons and 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 m...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 庞国芳范春林曹亚飞常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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