Determination of Organophosphorous Pesticides in Blood Using Microextraction in Packed Sorbent and Gas Chromatography-Tandem Mass Spectrometry

作者：Santos C; Oppolzer D; Goncalves A; Barroso M; Gallardo E^*

来源：Journal of Analytical Toxicology, 2018, 42(5): 321-329.

DOI：10.1093/jat/bky004

The aim of our work was to develop a method for the determination of six organophosphorous pesticides (Ops) (azynphos-ethyl (AZP), diazinon (DZN), chlorpyrifos (CLP), chlorfenvinfos (CLF), parathionethyl (PRT) and quinalphos (QLP)) in whole blood using microextraction by packed sorbent (MEPS) and analysis by gas chromatography-tandem mass spectrometry (GC-MS/MS). The optimization of the MEPS procedure was performed using a design of experiments (DOE) approach, assessing different factors that significantly affected the extraction efficiency. Ultimately, the number of sample strokes, wash volume, percentage of 2-propanol in the wash solvent and the number of elution strokes were successfully optimized using a response surface methodology (RSM). The developed and optimized method was fully validated according to international guidelines. Linearity was established from 2.5 to 50 mu g/mL for AZP and from 0.5 to 50 mu g/mL for the remaining compounds, with coefficients of determination (R-2) higher than 0.99 in all cases. The lower limit of quantification were 2.5 mu g/mL (AZP) and 0.5 mu g/mL (remaining compounds). Recoveries ranged from 61% to 77%. Intraand inter-day precision and accuracy were considered adequate according to the guidelines. This is the first method employing MEPS as a sample preparation procedure for the analysis of these OPs in whole blood.

• 出版日期2018-6