GC-Q-TOF/MS detection technology for 708 kinds of pesticide residues in melon fruit

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

Inactive Publication Date: 2016-06-08
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Abstract
  • Description
  • Claims
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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 kinds of pesticide residues in melon fruit
  • GC-Q-TOF/MS detection technology for 708 kinds of pesticide residues in melon fruit
  • GC-Q-TOF/MS detection technology for 708 kinds of pesticide residues in melon fruit

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 pesticide residues in fruits and vegetables provided by the present invention

[0088] (1) Weigh 10g of Hami melon samples from Urumqi 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 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.

[0089](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 ne...

Embodiment 2

[0097] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in fruits and vegetables provided by the present invention

[0098] According to the method in Example 1, the pesticide residues in the same batch of Hami melon samples are detected, the difference is that the pretreatment steps are as follows:

[0099] (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 o...

Embodiment 3

[0106] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in fruits and vegetables provided by the present invention

[0107] The pesticide residues in melons and fruits were detected according to the method in Example 1, except that the samples were watermelon samples in Beijing.

[0108] Collected 10 commercially available watermelon samples in Beijing area, and detected 2 kinds of pesticide residues, with a total of 8 frequencies, involving 8 samples. The specific results are shown in Table 3.

[0109] table 3

[0110]

[0111] Take isoxaflutole, which has a relatively high detection frequency, as an example: image 3 As shown, 4 fragment ion information were detected in watermelon, searched in the database, and compared with isoxaflutole, the matching scores of the 4 fragment ions were all above 90 points, and the retention time deviation was within 0.008min, the fragment with the highest abundance The ion...

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Abstract

The invention relates to the field of pesticide residue detection, and provides a detection method for screening 708 kinds of pesticide residues in melon fruit. The detection method comprises the following steps: acquiring a fragment ion full-scan mass spectrogram under specified conditions of pesticide standards in a GC-Q-TOF/MS level-one mode to obtain chemical molecular formulae, retention time, precise fragment ion mass numbers and ion abundance ratios of pesticides; importing the chemical molecular formulae, the retention time, the precise fragment ion mass numbers and the ion abundance ratios of the pesticides into PCDL software; correlating the chemical molecular formulae, the retention time, the precise fragment ion mass numbers and the ion abundance ratios of the pesticides with corresponding pesticide information to form a database; measuring full spectrum data of a sample to be detected under the same set conditions to obtain the full spectrum data; retrieving a detection result of the sample in a precise mass database to accurately authenticate the detected pesticides meeting an authentication basis to obtain pesticide residue varieties of the melon fruit. According to the detection method for screening 708 kinds of pesticide residues in the melon fruit, the pesticide residues in the melon fruit are detected by the detection method established by utilizing GC-Q-TOF/MS high resolution mass spectrum; preferably, a specified pre-treatment is combined; the detection method has the characteristics of quickness, high throughput, high precision and high reliability. A standard substance is not required for contrasting, and 708 pesticides in the melon fruit are detected and confirmed qualitatively.

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 melons and fruits by applying GC-Q-TOF / MS. Background technique [0002] Fruits and vegetables are closely related to people's lives, especially the nutritional value of melons and fruits (watermelon, cantaloupe, cantaloupe and muskmelon, etc.) are favored by consumers. However, at present, there are more than 1,100 kinds of pesticides and chemicals that may be used in the cultivation, growth and preservation of melons and fruits. However, with the widespread use of pesticides, irregular behaviors such as excessive use, abuse and misuse have also occurred, making pesticide residues in agricultural products, which poses a potential threat to human health, and also has a negative impact on the import and export of agricultural products. adverse effects. [0003] As early as 1976, the World Health Organi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 庞国芳范春林胡雪艳常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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