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GC-Q-TOF/MS detection technology for 708 pesticide residues in leaf vegetables

A GC-Q-TOF and leafy vegetable technology, applied in the field of pesticide residue detection, can solve the problems of high price, valid period of only 2-3 years, and loopholes in food safety monitoring, so as to save costs, save testing costs, and improve work efficiency effect

Inactive Publication Date: 2016-06-01
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 2-3 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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  • GC-Q-TOF/MS detection technology for 708 pesticide residues in leaf vegetables
  • GC-Q-TOF/MS detection technology for 708 pesticide residues in leaf vegetables
  • GC-Q-TOF/MS detection technology for 708 pesticide residues in leaf vegetables

Examples

Experimental program
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Effect test

Embodiment 1

[0090]This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in leafy vegetables provided by the present invention

[0091] (1) Weigh 10g of lettuce sample from Chengdu area (accurate to 0.01g), add 40mL of 1% acetic acid in acetonitrile solution to an 80ml centrifuge tube, use a high-speed homogenizer at 13500r / min, homogenize and extract for 1min, add 1g of chlorinated Sodium, 4g of anhydrous magnesium sulfate, shake for 5min, centrifuge at 4200r / min for 5min, take 20mL of supernatant, condense to about 1mL by rotary evaporation in a 40°C water bath, and wait for purification.

[0092] (2) 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 effluent. When the liquid level reaches the top of sodium sulfate, quickly transfer the concentrated sample solution to the SPE column, and then connect a new Heart b...

Embodiment 2

[0100] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in leafy vegetables provided by the present invention

[0101] According to the method in Example 1, the pesticide residues in the same batch of lettuce samples are detected. The difference is that the pretreatment steps are as follows:

[0102] (1) Accurately weigh 10.00g of sample into a centrifuge tube, add 50mL of water, and shake until the sample is fully soaked by water. After freezing for 10 min, pipette 50 mL of acetonitrile into a centrifuge tube, then place the centrifuge tube on a vortex mixer and vibrate at 2000 rpm for 1 min. Keep the centrifuge tube at -10°C for 10 minutes, then add 20g of anhydrous magnesium sulfate, 5g of sodium chloride, 5g of sodium citrate and 2.5g of sodium dihydrogen citrate into the centrifuge tube, and immediately place it on a vortex mixer , shake at 2000rpm for 2min, then centrifuge at 4000rpm for 10min to obtain su...

Embodiment 3

[0109] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in leafy vegetables provided by the present invention

[0110] The detection of pesticide residues in leafy vegetables was carried out according to the method in Example 1, except that the samples were celery samples from Chengdu area.

[0111] Collected 11 commercially available celery samples in Chengdu area, and detected 19 kinds of pesticide residues, with a total of 34 frequencies, involving 11 samples. The specific results are shown in Table 3.

[0112] table 3

[0113]

[0114]

[0115] Take Carbofuran, which has a high detection frequency, as an example: image 3 As shown, 6 fragment ions were detected in celery, searched in the database, and compared with carbofuran, the matching scores of 6 fragment ions were all above 91 points, and the retention time deviation was within 0.01min. The fragment ion with the highest abundance The quality dev...

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Abstract

The invention relates to the field of detection of pesticide residues and provides a detection method for screening 708 pesticide residues in leaf vegetables. In the GC-Q-TOF / MS first-class mode, a fragment ion full-scanning mass spectrum on the specified conditions of a pesticide standard, the chemical formula, the retention time, the fragment ion accurate mass number and the ion abundance ratio of pesticide are obtained, guided into PCDL software and related to corresponding pesticide information to form a database, and full-spectrum data of samples to be tested is determined on the identical set condition to obtain full-spectrum data. A sample measuring result is retrieved through a precise mass database, the detected pesticide meeting the identification basis is accurately identified, and pesticide residue varieties in leaf vegetables are obtained. The detection method built by applying the GC-Q-TOF / MS high resolution mass spectrum is used for detecting pesticide residues in leaf vegetables, specified pretreatment is preferentially combined, and the advantages that detection is rapid and high in throughput, precision and reliability are achieved. No standard is used as a contrast, and meanwhile 708 pesticides in the leaf vegetables are qualitatively detected and confirmed.

Description

technical field [0001] The invention relates to the field of pesticide residue detection, in particular to a detection method for screening 708 kinds of pesticide residues in leafy vegetables by using GC-Q-TOF / MS. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 庞国芳范春林李岩常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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