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LC-MS-MS (liquid chromatogram tandem mass spectrum) detecting method for residual quantity of mandipropamid in vegetables and dried fruits

A technology of LC-MS-MS and mandipropamid, which is applied in the field of detection of mandipropamid residues, achieving good repeatability, high sensitivity and avoiding matrix interference

Inactive Publication Date: 2016-07-13
INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no LC-MS-MS method that uses liquid chromatography-mass spectrometry to detect mandipropamid residues in various vegetables and dried fruits with complex matrices, and has wide adaptability, high sensitivity, good repeatability, and accurate qualitative and quantitative analysis. See the report

Method used

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  • LC-MS-MS (liquid chromatogram tandem mass spectrum) detecting method for residual quantity of mandipropamid in vegetables and dried fruits
  • LC-MS-MS (liquid chromatogram tandem mass spectrum) detecting method for residual quantity of mandipropamid in vegetables and dried fruits
  • LC-MS-MS (liquid chromatogram tandem mass spectrum) detecting method for residual quantity of mandipropamid in vegetables and dried fruits

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Experimental program
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Effect test

Embodiment 1

[0048] LC-MS-MS detection of mandipropamid residues in embodiment 1 tomato:

[0049] (1) Sample preparation:

[0050] Divide the collected tomato sample to 500g according to the quartering method, divide the sample into two parts of 2×200g, pulverize it with a food processor, and store it in a freezer at -20°C.

[0051] (2) Extraction and purification:

[0052] Weigh 5.0 g of the prepared tomato sample into a 50 mL centrifuge tube, add 10 ml of acetonitrile, homogenize at high speed for 2 min, add 2 g of NaCl, and shake vigorously for 1 min. Take the upper acetonitrile phase and centrifuge, take 1mL of the supernatant and add 1mL of methanol and water mixed solution (volume ratio 1:1) to pass through a 0.2μm nylon microporous filter membrane, and the obtained liquid phase is the sample to be tested.

[0053] (3) Preparation of standard working solution:

[0054] Treat the tomato matrix blank sample without mandipropamid according to the above steps (1) and (2) to obtain the...

Embodiment 2

[0075] LC-MS-MS detection of mandipropamid residues in embodiment 2 dried peppers:

[0076] (1) Sample preparation:

[0077] Divide the collected dried chili sample into 500g according to the quartering method, divide the sample into two parts of 2×200g, pulverize it with a food processor, and store it in a freezer at -20°C.

[0078] (2) Extraction and purification:

[0079] Weigh 5.0 g of the prepared dried pepper sample into a 50 mL centrifuge tube, add 10 ml of acetonitrile, homogenize at high speed for 2 min, add 2 g of NaCl, and shake vigorously for 1 min. Take the upper acetonitrile phase and centrifuge, take 1mL of the supernatant and add 1mL of methanol and water mixed solution (volume ratio 1:1) to pass through a 0.2μm nylon microporous filter membrane, and the obtained liquid phase is the sample to be tested.

[0080] (3) Preparation of standard working solution:

[0081] Treat the dry pepper matrix blank sample without mandipropamid according to the above steps (...

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Abstract

The invention discloses an LC-MS-MS (liquid chromatogram tandem mass spectrum) detecting method for residual quantity of mandipropamid in vegetables and dried fruits and belongs to the technical field of pesticide residual quantity detection.The method comprises the steps that an acetonitrile solution is used for extracting mandipropamid remained in a sample in a homogeneity mode, LC-MS-MS detecting is conducted after the extracting solution is dispersed and purified, a correction standard curve is established through a blank matrix solution not containing pesticide to be detected, and quantitation is conducted through an external standard method.According to the method, the average recovery rate is 85.0-94.6%, the relative standard deviation (RSD) is 0.86-2.89%, the detection limit is 0.003 mg / kg, and the quantitative detection limit is 0.01 mg / kg.The method has the advantages that operation is easy, convenient and quick, sensitivity is high, repeatability is good, and quality and quantitation are accurate.The uniform limit technical requirement for the 0.01 mg / kg residual limit can be met, and strong technical support is provided for guaranteeing people food safety in China and health development of export abroad trades.

Description

technical field [0001] The present invention relates to a method for detecting the residual amount of mandipropamid, more specifically to a method for detecting the residual amount of mandipropamid in vegetables and dried fruits by LC-MS-MS (liquid chromatography-tandem mass spectrometry), The invention belongs to the technical field of pesticide residue detection. Background technique [0002] The chemical name of mandipropamid is 2-(4-chlorophenyl)-N-[2-(3-methoxy-4-prop-2-ynyloxy-phenyl)-ethyl]-2 -Prop-2-ynyloxy-acetamide, the English chemical name is 2-(4-chlorophenyl)-N-[2-(3-methoxy-4-prop-2-ynyloxy-phenyl)-ethyl]-2- prop-2-ynyloxy-acetamide. The CAS accession number is [374726-62-2]. Molecular formula: C23H22ClNO4, relative molecular mass: 411.9. The chemical structural formula is as follows: [0003] [0004] Physical and chemical properties: Light brown powder, melting point 96.4°C~97.3°C. It starts thermal decomposition at about 200°C boiling point. Vapor...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 李慧冬陈子雷董崭范文静张文君朱倩
Owner INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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