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HPLC-MS/MS detection method of fluopicolide and metabolic products of fluopicolide

A technology for fluopicolide and its metabolites, which is applied in the field of HPLC-MS/MS detection of fluopicolide and its metabolites, can solve the problems of no M2 detection related reports, shorten the sample analysis cycle, and achieve selectivity Good, high-sensitivity effect

Active Publication Date: 2018-09-28
INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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Problems solved by technology

[0006] Most of the reported fluopicolide residue tests are for fluopicolide parent, as long as very few studies have carried out the detection of fluopicolide parent and M1 at the same time, there is no report on the detection of M2

Method used

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  • HPLC-MS/MS detection method of fluopicolide and metabolic products of fluopicolide
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  • HPLC-MS/MS detection method of fluopicolide and metabolic products of fluopicolide

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Embodiment Construction

[0039] 1 Materials and methods

[0040] 1.1 Test materials

[0041] 99.2% fluopicolide, 96.2% M-01 (2,6-dicholrobenzamide) and 98.5% M-02 (3-chloro-5-(trifl uoromethyl)pyridine-2-carboxylic acid) Bayer Crop Science ( China) Co., Ltd.; acetonitrile: chromatographically pure, FISHER; methanol: superior grade, FISHER; formic acid: chromatographically pure, CNW; ultrapure water: Wahaha; QuEChERS material: Agilent.

[0042] 1.2 Main instruments

[0043] 1290-G6460C high performance liquid chromatography-tandem electrospray triple quadrupole mass spectrometer (Agilent, USA); G6460C mass spectrometry system (Agilent, USA); ultrasonic extractor (Kunshan Ultrasonic Instrument Co., Ltd.); high-speed homogenizer (Germany IKA WORK INC T25Basic); rotary evaporator (Heidolph LABOROTA 4001, Germany); high-speed centrifuge (Heal Force, Hong Kong); glass instruments commonly used in laboratories.

[0044] 1.3 Instrument testing conditions

[0045] 1.3.1 Fluopyram, metabolite M-01

[0046]...

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Abstract

The invention discloses an HPLC-MS / MS detection method of fluopicolide and metabolic products of fluopicolide. The method comprises the steps of taking and grinding a solid sample (an onion, soil andthe like), adding acetonitrile containing 0.2% formic acid for uniform mixing, performing homogenization through a high-speed homogenization machine, and ultrasound extraction and centrifugation at 20-30 DEG C, taking a supernate, adding the same volume of methanol aqueous solution at a concentration of 50%, performing filtration through a filtration membrane to form liquid to be detected, and qualitatively and / or quantitatively analyzing fluopicolide and the metabolic products M-01 and M-02 of fluopicolide for the liquid to be detected through a high performance liquid chromatography-triple quadrupole tandem mass spectrometer. The method is simple, convenient and easy to operate, and can meet requirements on quick detection and confirmation of a residual quantity of fluopicolide and the metabolic products M-01 and M-02 of fluopicolide in the onion and the soil, and provide a theoretical basis for safe and scientific use of fluopicolide for the onion and establishment of a maximum residue limit of fluopicolide in the onion in China.

Description

technical field [0001] The invention relates to a detection method, in particular to an HPLC-MS / MS detection method of fluopyram and its metabolites. Background technique [0002] Fluopicolide, the chemical name is 2,6-dichloro-N-[(3-chloro-5-trifluoromethyl-2-pyridyl)methyl]benzamide, and its structural formula is as follows. Fluopyram is a new type of benzamide fungicide with a unique mechanism of action developed by Bayer Crop Science. It is a fluorine-containing fungicide with a new mechanism of action. It has the characteristics of low toxicity, high drug efficacy and strong metabolic ability, and has high biological activity against oomycetes. It is mainly used to prevent and control common oomycete diseases on vegetables and grapes. [0003] [0004] At present, studies on the toxicology of fluopicolide mainly focus on fluopicolide parent (fluopicolide) and two main metabolites M-01 (2,6-dichlorobenzamide) and M-02 (3-chloro-5-(trifl uoromethyl)pyridine-2-carboxy...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 方丽萍陈子雷张文君丁蕊艳杜红霞李慧冬王晨晨
Owner INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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