title: Ruggedness and other performance characteristics of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in food crops.
abstract: Low-pressure gas chromatography-mass spectrometry (LP-GC-MS) using a quadrupole MS instrument was further optimized and evaluated for the fast analysis of multiple pesticide residues in food crops. Performance of two different LP-GC-MS column configurations was compared in various experiments, including ruggedness tests with repeated injections of pesticides in matrix extracts. The tested column configurations employed the same 3 m x 0.15 mm i.d. restriction capillary at the inlet end, but different analytical columns attached to the vacuum: (A) a 10 m x 0.53 mm i.d., 1 microm film thickness RTX-5 Sil MS column; and (B) a 10 m x 0.25 mm i.d., 0.25 microm film thickness DB-5MS column. Under the optimized conditions (compromise between speed and sensitivity), the narrower analytical column with a thinner film provided slightly (<1.1-fold) faster analysis of <5.5 min separation times and somewhat greater separation efficiency. However, lower detection limits for most of the tested pesticides in real extracts were achieved using the mega-bore configuration, which also provided significantly greater ruggedness of the analysis (long-term repeatability of analyte peak intensities, shapes, and retention times). Additionally, the effect of the increasing injection volume (1-5 microl) on analyte signal-to-noise ratios was evaluated. For the majority of the tested analyte-matrix combinations, the increase in sensitivity caused by a larger injection did not translate in the same gain in analyte detectability. Considering the costs and benefits, the injection volume of 2-3 microl was optimal for detectability of the majority of 57 selected pesticides in apple, carrot, lettuce, and wheat extracts.
authors.affiliation: USDA, Agricultural Research Service, Eastern Regional Research Center, Wyndmoor, PA 19038, USA.
authors.forename: Katerina
authors.initials: K
authors.lastname: Mastovská
authors.forename: Jana
authors.initials: J
authors.lastname: Hajslová
authors.forename: Steven J
authors.initials: SJ
authors.lastname: Lehotay
mesh_terms: D018556:Crops, Agricultural / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis*; D011312:Pressure; D012680:Sensitivity and Specificity
chemical_list: D010573:Pesticide Residues