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Rapid detection method for simultaneous determination of 34 pesticide residues in fruits and vegetables

A technology for pesticide residue detection, fruits and vegetables, applied in the field of pesticide detection, can solve the problems of unfavorable and rapid detection of pesticide residues in fruits and vegetables, unable to analyze at the same time, affecting the circulation of fruits and vegetables, etc., to shorten the working time, protect the environment, and reduce the amount of use.

Inactive Publication Date: 2018-05-11
浙江公正检验中心有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current relevant testing standards can only detect a few of them, and cannot be analyzed at the same time; for example, GB / T 20770-2008 can only detect 20 of the 34 types, and GB / T 23584-2009 can only detect 1 of the 34 types. NY / T 1453-2007 can only detect 7 of 34 types, NY / T 1720-2009 can only detect 2 of 34 types, GB 23200.34-2016 can only detect 15 of 34 types, SN / T 2560-2010 can only detect 4 of the 34 types, GB / T 20769-2008 can only detect 18 of the 34 types, etc.
Therefore, in the detection process, if all items need to be checked, different methods need to be adopted, and the work efficiency is very low, which is not conducive to the rapid detection of pesticide residues in fruits and vegetables, and affects the circulation of fruits and vegetables in the market

Method used

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  • Rapid detection method for simultaneous determination of 34 pesticide residues in fruits and vegetables
  • Rapid detection method for simultaneous determination of 34 pesticide residues in fruits and vegetables
  • Rapid detection method for simultaneous determination of 34 pesticide residues in fruits and vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Establishment of Chromatograms of 34 Kinds of Pesticide Residue Reference Substances

[0055] Include the following steps:

[0056] (1) Ultra-high performance liquid chromatography-mass spectrometry, mass spectrometry conditions

[0057] a Chromatographic conditions

[0058] Chromatographic column: using Agilent SB-C 18 Column (2.1×100mm, 1.8μm, USA)

[0059] Column temperature: 35°C;

[0060] Injection volume: 5μL; flow rate: 0.3mL / min;

[0061] Mobile phase A: 0.1% formic acid water; mobile phase B: acetonitrile=90~10:10~90 (volume ratio), gradient elution 0~3min, A changes from 90 to 50%; 3~5min, A changes from 50 10%; 5 ~ 8min to maintain A 10%; 8 ~ 10min, A changed from 10 to 90%.

[0062] b mass spectrometry conditions

[0063] Ion source: electrospray ion source (ESI); scan mode: positive ion;

[0064] Detection method: multiple reaction monitoring (MRM) acquisition;

[0065] Detector: Agilent 6460 triple quadrupole mass spectrometer equipped with ESI ion ...

Embodiment 2

[0077] The determination of 34 kinds of pesticide residue content in the apple sample of embodiment 2

[0078] Include the following steps:

[0079] (1) Preparation of test samples

[0080] Accurately weigh 5.00 g of the crushed apple sample, add 10 mL of extractant, homogenize for 1 min, add 2 g of sodium chloride and anhydrous magnesium sulfate respectively, continue homogenizing for 2 min, and then centrifuge at 4000 r / min for 5 min. Take 5mL of the supernatant to a straight tube, blow with nitrogen in a 40°C water bath until dry, add 2mL of 50% methanol aqueous solution to redissolve, vortex and mix well, add 50mg of PSA powder, 50mg of anhydrous magnesium sulfate, 50mg of florisil and 50mgC 18 powder, vortex again and pass through a 0.22μm filter membrane to obtain the test sample.

[0081] (2) Ultra-high performance liquid chromatography-mass spectrometry, mass spectrometry conditions

[0082] a Chromatographic conditions

[0083] Chromatographic column: using Agile...

Embodiment 3

[0093] Example 3 Determination of Pesticide Residues in Apple Samples Adding Concentration of 5.0 μg / kg of 34 Pesticide Residues

[0094] Include the following steps:

[0095] (1) Preparation of test samples

[0096] Accurately weigh 5.00 g of the negative apple sample processed by crushing in Example 2, and add 1.0 mL of mixed working solution with a concentration of 100.0 ng / mL to the sample, then the concentration of 34 pesticide residues in the apple sample is 5.0 μg / kg, follow-up treatment is the same as embodiment 2, obtains the test sample.

[0097] (2) Ultra-high performance liquid chromatography-mass spectrometry, mass spectrometry conditions

[0098] With embodiment 2.

[0099] (3) Determination

[0100] The test sample that the injection volume is 5 μ L carries out HPLC-MS / MS detection, obtains the total ion chromatogram (such as image 3 shown). According to the sample quality represented by the test sample, the content of 34 kinds of pesticide residues in t...

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Abstract

The invention relates to the field of pesticide detection, and aims at providing an LC-MS detection method for simultaneous determination of 34 pesticide residues in fruits and vegetables to achieve simultaneous analysis of the 34 pesticide residues without using multiple detection methods and to meet the requirements for rapid and efficient detection work. The invention also provides a sample pretreatment method for detecting the pesticide residues in the fruits and the vegetables, and the method has the advantages of spending little time and having a good extraction effect. According to thetechnical scheme, an extracting agent for sample pretreatment for detecting the pesticide residues in the fruits and the vegetables comprises, by weight, 0-8 parts of acetonitrile, 0-5 parts of acetone and 0-3 parts of 1-butyl-3-methylimidazol dicyanamide salt; the rapid detection method for the simultaneous determination of the 34 pesticide residues in the fruits and the vegetables includes the following steps of making a standard curve and detecting samples to be detected.

Description

technical field [0001] The invention relates to the field of pesticide detection, in particular to a method for simultaneously determining 34 kinds of pesticide residues in fruits and vegetables by liquid chromatography-mass spectrometry. Background technique [0002] With the development of agricultural industrialization, the production of agricultural products is increasingly dependent on exogenous substances such as pesticides, antibiotics and hormones. Pesticide residues exceeding the standard will affect the food safety of consumers, and in severe cases will cause consumers to become ill, develop abnormally, and even directly lead to poisoning death. In order to ensure food safety and strictly supervise the pesticide residues in food, one of the most effective methods is to strengthen the detection of pesticide residues in food. [0003] Carbofuran, methomyl, carbaryl, aldicarb, carbendazim, imidacloprid, methomyl, acetamiprid, pymetrozine, forchlorfenuron, propamocarb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王庆龄徐坤华许荣年杨琳裘钧陶杨娜秦芸桦
Owner 浙江公正检验中心有限公司
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