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GC-Q-TOF/MS detection technology of 708 pesticide residues in root vegetables and tuber vegetables

A GC-Q-TOF, rhizome technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high price, valid period of only 2-3 years, food safety monitoring loopholes, etc., to save costs and save testing cost, work efficiency improvement effect

Inactive Publication Date: 2016-04-20
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 root vegetables and tuber vegetables
  • GC-Q-TOF/MS detection technology of 708 pesticide residues in root vegetables and tuber vegetables
  • GC-Q-TOF/MS detection technology of 708 pesticide residues in root vegetables and tuber vegetables

Examples

Experimental program
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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 rhizomes and yam vegetables provided by the present invention

[0088] (1) The edible part of the commercially available carrot samples in Shenyang was chopped, mixed evenly, sealed, and marked. .

[0089] (2) Weigh 10g of the above carrot 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, extract the homogenate for 1min, and 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. Whe...

Embodiment 2

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

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

[0100] (1) The edible part of the carrot sample should be chopped, mixed evenly, sealed and marked. .

[0101] (2) Accurately weigh 10.00 g of the sample into a centrifuge tube, add 50 mL of water, and shake until the sample is fully saturated with 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 t...

Embodiment 3

[0108] This example is used to illustrate the GC-Q-TOF / MS detection method for screening 708 kinds of pesticide residues in rhizomes and yam vegetables provided by the present invention

[0109] The detection of pesticide residues in rhizome and yam vegetables was carried out according to the method in Example 1, except that the samples were radish samples from Changchun area.

[0110] Seven radish samples were collected in Changchun area, and 3 pesticide residues were detected, with a total of 3 frequencies, involving 3 samples. The specific results are shown in Table 3.

[0111] table 3

[0112]

[0113] Take diphenylamine, which is detected frequently, as an example: image 3 As shown, 4 pieces of fragment ion information are detected in the pepper, searched with the database, and compared with diphenylamine, the matching scores of the 4 fragment ions are all above 85 points, and the retention time deviation is within 0.035min (such as Figure 4 Shown), it can be confi...

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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 root vegetables and tuber vegetables. The method comprises the steps of collecting full-scan mass spectrum of fragment ions under specified requirements of pesticide standards in a GC-Q-TOF / MS first-class mode and obtaining chemical formula, retention time, accurate mass number of fragment ions and ion abundance ratio of a pesticide, importing PCDL software, correlating with the corresponding pesticide information to form a database, measuring full spectrum data of a sample to be detected under the same setting condition, so as to obtain the full spectrum data; performing accurate quality database retrieval on a sample determine result, accurately identifying the detected pesticide accorded with the identification basis, so as to obtain the types of pesticide residues in the in root vegetables and tuber vegetables. A detection method established by a GC-Q-TOF / MS high resolution mass spectrum is adopted to detect the pesticide residues in the root vegetables and the tuber vegetables, specific pretreatment is preferably combined, and the characteristics of speediness, high throughput, high precision and high reliability detection are achieved. A standard substance as contrast is not required, and meanwhile the 708 pesticides in the root vegetables and the tuber vegetables are subjected to qualitative detection and confirmation.

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 rhizome and yam 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 root and tuber vegetables (potatoes, radishes, carrots, taro, purple potatoes, bellflowers, sweet potatoes, yacon, ginger and yams, etc.) are favored by consumers . This kind of vegetable is mainly starch, with high sugar content, such as purple sweet potato, taro, potato, yam, etc., which can partially replace the staple food. Other nutrients are different, such as iodine, bromine, amylase in radish; potassium salt and vitamin C in potato; high carotene in carrot. However, at present, there are more than 1100 kinds of pesticides and chemicals that may be used in the planting, growth and preservation of rhizome and yam vegetable...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 庞国芳范春林李晓颍常巧英
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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