Unlock instant, AI-driven research and patent intelligence for your innovation.

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

A Q-TOF, pesticide residue technology, applied in measuring devices, material analysis by electromagnetic means, instruments, etc., can solve problems such as high price, loopholes in food safety monitoring, and only 2 or 3 years of validity, achieving a large amount of information. Effect

Inactive Publication Date: 2016-07-06
CHINESE ACAD OF INSPECTION & QUARANTINE
View PDF2 Cites 11 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in leaf vegetables
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in leaf vegetables
  • LC-Q-TOF/MS detection technology for 544 pesticide residues in leaf vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] An implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in leafy vegetables (taking celery as an example) includes the following steps:

[0066] 1. Specific steps of sample pretreatment technology:

[0067] 1.1 Take the edible part of the celery sample, chop it up, mix it evenly, seal it, and mark it;

[0068] 1.2 Weigh 10g of celery 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.

[0069] 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 d...

Embodiment 2

[0099] Example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in leafy vegetables (taking mustard greens 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 leafy mustard samples in a provincial capital city: 12 commercial leafy mustard samples were collected in a provincial capital city, and 544 pesticide residu...

Embodiment 3

[0107] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in leafy vegetables (taking lettuce 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 lettuce samples in a provincial capital city: 9 samples of lettuce sold in a provincial capital city were collected, and 544 kinds of pesticide resi...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides an LC-Q-TOF / MS detection technology for 544 pesticide residues in leaf vegetables. 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 leaf vegetables 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 leaf 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 leafy 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N30/02
CPCG01N27/62G01N30/02G01N2030/027
Inventor 庞国芳范春林康健常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE