4.7 Article

Applications of LC/ESI-MS/MS and UHPLC QqTOF MS for the determination of 148 pesticides in fruits and vegetables

Journal

ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 396, Issue 4, Pages 1513-1538

Publisher

SPRINGER HEIDELBERG
DOI: 10.1007/s00216-009-3331-6

Keywords

LC/ESI-MS/MS; UHPLC QqTOF; Pesticides; Fruits; Vegetables; Measurement uncertainty

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This paper presented the applications of liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) and ultra-high-pressure liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry (UHPLC QqTOF MS) for the determination of 148 pesticides in fruits and vegetables. Pesticides were extracted from fruits and vegetables using a buffered QuEChERS method. Quantification was achieved using matrix-matched standard calibration curves with isotopically labeled standards or a chemical analog as internal standards in an analytical range from 5 to 500 mu g/kg. The method performance parameters including overall recovery, intermediate precision, and measurement uncertainty were evaluated according to a statistically designed experiment, i.e., a nested design. For LC/ESI-MS/MS, 95% of the pesticides had recoveries between 81% and 110%; 97% had an intermediate precision a parts per thousand currency sign20%; and 95% (in fruits) or 93% (in vegetables) showed measurement uncertainty a parts per thousand currency sign40%. Compared to LC/ESI-MS/MS, UHPLC QqTOF MS showed a relatively poor repeatability and large measurement uncertainty. About 93% (in fruits) or 94% (in vegetables) of the pesticides had recoveries between 81% and 110%; 86% (in fruits) or 90% (in vegetables) had an intermediate precision a parts per thousand currency sign20%; and 79% (in fruits) or 88% (in vegetables) showed measurement uncertainty a parts per thousand currency sign40%. LC/ESI-MS/MS proved to be the first choice for quantification or pre-target analysis due to its superior sensitivity and good repeatability. UHPLC QqTOF MS provided accurate mass measurement and isotopic patterns, and was an ideal tool for post-target screening and confirmation.

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