Analysis of pesticides in food products using SFE-SFC-MSMS

Tuesday, November 29, 2016

Author: Sigrid Baumgarten


Keywords: SFE-SFC-MSMS, pesticide residues, Supercritical Fluid Extraction (SFE), Supercritical Fluid Chromatography (SFC), mass spectrometry, QuEChERS, hydrophilic interaction chromatography



1. Abstract

The use of an online system combining Supercritical Fluid Extraction (SFE) and Su­percritical Fluid Chromatography (SFC) with tandem Mass Spectrometry for the anal­ysis of pesticide residues in food products is introduced in this study. In addition, SFE of organochlorine pesticides was performed for subsequent analysis by GC-MS/MS. SFC was proven to be a powerful technique for the separation of a wide range of pesticides with different chemical structures, polarities and molecular weights.

100 pesticides were extracted from different food matrices and analyzed using the online SFE-SFC-MS/MS system. The entire process was characterized by good re­peatability in the concentration range 1 to 10 ng/g. LOQs ranged from 0.1 to 10 μg/L

The system was configured to enable automated switching to offline extraction to perform analysis with either SFC or GC-MS. Offline SFE and analysis by GC-MS of or­ganochlorine pesticides was accomplished with good accuracy (recoveries between 80 and 125%) for the majority of analytes.


1. Introduction


The multi-residue determination of pesticides is ex­tremely challenging due to the uncertainty concerning the adverse effects that these residues may have on human health after a prolonged exposure at low con­centration levels. Consequently, stricter food safety regulations are being enforced around the world, placing pesticide analysis laboratories under increas­ing pressure to expand the list of target pesticides and to detect analytes at lower concentrations [1].

GC-MS and LC-MS are two main techniques used for pesticide residue analysis. Due to the wide range of physiochemical properties of pesticides, two sep­arate analyses by GC-MS/MS and LC-MS/MS are often required. In general, LC is favored for polar and non-volatile compounds, while GC is used for volatile compounds [2]. There has been an increasing de­mand for a complex system able to analyze multiple pesticides with a wide range of properties simultane­ously, also including a sample preparation unit.

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