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GC-Q-TOF/MS detection technology of 708 pesticide residues in legume vegetables

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

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 2-3 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 of 708 pesticide residues in legume vegetables
  • GC-Q-TOF/MS detection technology of 708 pesticide residues in legume vegetables
  • GC-Q-TOF/MS detection technology of 708 pesticide residues in legume vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in legume vegetables provided by the present invention

[0088] (1) The edible part of the bean sample sold in Beijing area was chopped, mixed, sealed, and marked.

[0089](2) Weigh 10g of the above carob sample (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 sodium chloride , 4g of anhydrous magnesium sulfate, shake for 5min, centrifuge at 4200r / min for 5min, take 20mL of the supernatant, concentrate it to about 1mL by rotary evaporation in a water bath at 40°C, and wait for purification.

[0090] (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 effluent. When the liquid level reaches the top of sodi...

Embodiment 2

[0098] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in legume vegetables provided by the present invention

[0099] According to the method in Example 1, the pesticide residues in the same batch of beans samples are detected, the difference is that the pretreatment steps are as follows:

[0100] (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 sup...

Embodiment 3

[0107] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in legume vegetables provided by the present invention

[0108] The detection of pesticide residues in legume vegetables was carried out according to the method in Example 1, the difference is that the sample was a bean sample in Tianjin area.

[0109] 17 samples of beans sold in the Tianjin area were collected, and 24 kinds of pesticide residues were detected, with a total of 76 frequencies involving 16 samples. The specific results are shown in Table 3.

[0110] table 3

[0111]

[0112] Take wezaling, which has a high detection frequency, as an example, such as image 3 As shown, 4 fragment ions were detected in beans, searched in the database, and compared with Vezalin, the molecular weight deviation scores of the 4 fragment ions were all above 95 points, and the retention time deviation was within 0.008min, the fragment with the highest abundance T...

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Abstract

The invention relates to the field of pesticide residue detection and provides a detection method for screening 708 pesticide residues in legume vegetables. The method includes the steps of: a) under a first-stage mode of GC-Q-TOF / MS, collecting a fragment ion full-scanning mass spectrogram of pesticide reference substances under certain conditions to obtain a chemical formula, retention time, accurate mass numbers of fragment ions, and ion abundance ratio of the pesticide; b) introducing the data to PCDL software, correlating the data with corresponding pesticide information to obtain a database; c) under the same preset conditions, detecting the full-spectrum data of the to-be-detected samples; and d) performing accurate mass database retrieval to the sample detection results, and accurately identifying the detected pesticide satisfying identification basis to obtain the types of the pesticide residues in the legume vegetables. By means of the GC-Q-TOF / MS high-resolution mass spectrum, the detection method can detect the pesticide residues in the legume vegetables, preferably, with combination of special pre-treatments, so that the method is quick, high-throughput, high-precision and high-reliability. The method is free of a reference substance and can be used for qualitatively detecting and identifying the 708 pesticides in legume vegetables.

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 beans and vegetables by using GC-Q-TOF / MS. Background technique [0002] Fruits and vegetables are closely related to people's lives, especially the nutritional value of legume vegetables (peas, lentils, kidney beans, edamame, beans, vegetable soybeans, edible peas, cowpeas, etc.) is favored by consumers. Most legume vegetables contain higher plant protein, carbohydrates, vitamins and inorganic salts than other vegetables. The content of vitamins is higher in B vitamins, and the content of vitamin B is the highest. However, there are more than 1100 kinds of pesticides and chemicals that may be used in the planting, growth and preservation of bean vegetables at present. However, with the widespread use of pesticides, irregular behaviors such as excessive use, abuse and misuse have also occurred, making...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N30/02
CPCG01N27/62G01N30/02G01N2030/025
Inventor 庞国芳范春林李岩胡雪艳
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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