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Determination of 23 organochlorine pesticides in animal feeds by GC-MS/MS after QuEChERS with EMR-Lipid clean-up

Abstract

A method has been developed to analyse 23 organochlorine pesticides in animal feed. These persistent pesticides include DDTs, dieldrin, and chlordane. All were legislated by Commission Regulation (EC)396/2005. The variation in the feed composition matrix was reduced by using a QuEChERS method, that includes freezing with CaCl2, based on a clean-up with Enhanced Matrix Removal—Lipid (EMR-L). The method based in two steps: screening and quantification, has been developed and validated following the SANTE/11813/2017 criteria. The analytes were extracted and analysed by gas chromatography coupled to a triple quadrupole mass spectrometry (GC-QQQ). Separation is achieved in 22 min. Satisfactory results were obtained in screening method validation. This was tested by evaluating the detection and identification of analytes in spiked samples on 21 different feeds. Excellent linearity and good sensitivity were achieved in the quantification method validation based on calibration by standard addition, which reduces the matrix effect. Recoveries between 70-120% at the quantification limit of 0.005 mg/kg were also obtained. In Catalonia, 200 samples of various feed matrix from agriculture production were analysed with good results, obtaining only 1% positives. The main positive pesticide was DDE; its presence in the sample could be due to the persistence of this family of pesticides in the environment.

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Publication details

The article was received on 28 Jun 2018, accepted on 02 Oct 2018 and first published on 03 Oct 2018


Article type: Paper
DOI: 10.1039/C8AY01436A
Citation: Anal. Methods, 2018, Accepted Manuscript
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    Determination of 23 organochlorine pesticides in animal feeds by GC-MS/MS after QuEChERS with EMR-Lipid clean-up

    L. Sanchez Costa, P. Rodríguez Martínez and M. Medina Sala, Anal. Methods, 2018, Accepted Manuscript , DOI: 10.1039/C8AY01436A

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