title: Fast gas chromatographic residue analysis in animal feed using split injection and atmospheric pressure chemical ionisation tandem mass spectrometry.
abstract: Significant speed improvement for instrumental runtime would make GC–MS much more attractive for determination of pesticides and contaminants and as complementary technique to LC–MS. This was the trigger to develop a fast method (time between injections less than 10 min) for the determination of pesticides and PCBs that are not (or less) amenable to LC–MS. A key factor in achieving shorter analysis time was the use of split injection (1:10) which allowed the use of a much higher initial GC oven temperature. A shorter column (15 m), higher temperature ramp, and higher carrier gas flow rate (6 mL/min) further contributed to analysis-time reduction. Chromatographic resolution was slightly compromised but still well fit-for-purpose. Due to the high sensitivity of the technique used (GC–APCI-triple quadrupole MS/MS), quantification and identification were still possible down to the 10 μg/kg level, which was demonstrated by successful validation of the method for complex feed matrices according to EU guidelines. Other advantages of the method included a better compatibility of acetonitrile extracts (e.g. QuEChERS) with GC, and a reduced transfer of co-extractants into the GC column and mass spectrometer.
authors.affiliation: RIKILT-Wageningen UR, Akkermaalsbos 2, 6708 WB Wageningen, The Netherlands. Electronic address: marc.tienstra@wur.nl.
authors.forename: M
authors.initials: M
authors.lastname: Tienstra
authors.affiliation: RIKILT-Wageningen UR, Akkermaalsbos 2, 6708 WB Wageningen, The Netherlands; Research Institute for Pesticides and Water, University Jaume I, 12071 Castellón, Spain.
authors.forename: T
authors.initials: T
authors.lastname: Portolés
authors.affiliation: Research Institute for Pesticides and Water, University Jaume I, 12071 Castellón, Spain.
authors.forename: F
authors.initials: F
authors.lastname: Hernández
authors.affiliation: RIKILT-Wageningen UR, Akkermaalsbos 2, 6708 WB Wageningen, The Netherlands.
authors.forename: J G J
authors.initials: JGJ
authors.lastname: Mol
mesh_terms: D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D001274:Atmospheric Pressure; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry; D010575:Pesticides / Q000032:analysis; D053719:Tandem Mass Spectrometry
chemical_list: D010575:Pesticides