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Simultaneous determination of 106 pesticides in nuts by LC-MS/MS using freeze-out combined with dispersive solid-phase extraction purification. 2017

Jingjing Wang, and Zhiguo Gong, and Tingting Zhang, and Shun Feng, and Jide Wang, and Yi Zhang
Key Laboratory of Oil and Gas Fine Chemicals, Ministry of Education & Xinjiang Uygur Autonomous Region, College of Chemistry and Chemical Engineering Xinjiang University, Urumqi, China.

As a result of the low water content and high fat matrices in nuts, it is very difficult to simultaneously determine multi-pesticides in trace levels. Here, a sample pretreatment method was developed in which, microwave-assisted solvent extraction was firstly used to extract pesticides, and then a two-step cleanup method was conducted combining freeze-out with dispersive solid-phase extraction to remove the lipidic matrix. By this way, 106 pesticides were simultaneously determined in the complicated nut sample by using an ultra-high pressure liquid chromatography coupled with a tandem mass spectrometer. Average recoveries were 75.3-119.3% with relative standard deviations < 14% at three concentration levels. The limits of detection and quantification were in the ranges of 0.3-3.0 and 1.0-10.0 μg/kg, respectively. Furthermore, the method was successfully applied to the determination of pesticides in 180 commercial nut samples.

UI MeSH Term Description Entries
D009754 Nuts Botanically, a type of single-seeded fruit in which the pericarp enclosing the seed is a hard woody shell. In common usage the term is used loosely for any hard, oil-rich kernel. Of those commonly eaten, only hazel, filbert, and chestnut are strictly nuts. Walnuts, pecans, almonds, and coconuts are really drupes. Brazil nuts, pistachios, macadamias, and cashews are really seeds with a hard shell derived from the testa rather than the pericarp. Nut
D010575 Pesticides Chemicals used to destroy pests of any sort. The concept includes fungicides (FUNGICIDES, INDUSTRIAL); INSECTICIDES; RODENTICIDES; etc. Pesticide
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D005506 Food Contamination The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage. Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D052616 Solid Phase Extraction An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods. Extraction, Solid Phase,Extractions, Solid Phase,Solid Phase Extractions
D053719 Tandem Mass Spectrometry A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection. Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem

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