PMID- 29373695 OWN - NLM STAT- MEDLINE DCOM- 20181015 LR - 20191210 IS - 1945-2403 (Electronic) IS - 0146-4760 (Linking) VI - 42 IP - 5 DP - 2018 Jun 1 TI - Determination of Organophosphorous Pesticides in Blood Using Microextraction in Packed Sorbent and Gas Chromatography-Tandem Mass Spectrometry. PG - 321-329 LID - 10.1093/jat/bky004 [doi] AB - 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), parathion-ethyl (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 mug/mL for AZP and from 0.5 to 50 mug/mL for the remaining compounds, with coefficients of determination (R2) higher than 0.99 in all cases. The lower limit of quantification were 2.5 mug/mL (AZP) and 0.5 mug/mL (remaining compounds). Recoveries ranged from 61% to 77%. Intra- and 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. FAU - Santos, C AU - Santos C AD - Centro de Investigacao em Ciencias da Saude (CICS-UBI), Universidade da Beira Interior, Av. Infante D. Henrique, 6201-556 Covilha, Portugal. AD - Laboratorio de Farmaco-Toxicologia, UBIMedical, Universidade da Beira Interior, EM506, 6201-556 Covilha, Portugal. FAU - Oppolzer, D AU - Oppolzer D AD - Centro de Investigacao em Ciencias da Saude (CICS-UBI), Universidade da Beira Interior, Av. Infante D. Henrique, 6201-556 Covilha, Portugal. FAU - Goncalves, A AU - Goncalves A AD - Centro de Investigacao em Ciencias da Saude (CICS-UBI), Universidade da Beira Interior, Av. Infante D. Henrique, 6201-556 Covilha, Portugal. FAU - Barroso, M AU - Barroso M AD - Instituto Nacional de Medicina Legal e Ciencias Forenses-Delegacao do Sul, Rua Manuel Bento de Sousa, 3, 1169-201 Lisboa, Portugal. FAU - Gallardo, E AU - Gallardo E AD - Centro de Investigacao em Ciencias da Saude (CICS-UBI), Universidade da Beira Interior, Av. Infante D. Henrique, 6201-556 Covilha, Portugal. AD - Laboratorio de Farmaco-Toxicologia, UBIMedical, Universidade da Beira Interior, EM506, 6201-556 Covilha, Portugal. LA - eng PT - Journal Article PT - Validation Study PL - England TA - J Anal Toxicol JT - Journal of analytical toxicology JID - 7705085 RN - 0 (Organophosphates) RN - 0 (Organophosphorus Compounds) RN - 0 (Organothiophosphorus Compounds) RN - 0 (Pesticides) RN - 0 (Solvents) RN - ND2M416302 (2-Propanol) SB - IM MH - 2-Propanol/chemistry MH - Analytic Sample Preparation Methods MH - Blood Banks MH - Calibration MH - Drug Stability MH - Gas Chromatography-Mass Spectrometry MH - Humans MH - Least-Squares Analysis MH - Limit of Detection MH - Molecular Structure MH - Organophosphates/*blood/chemistry/isolation & purification MH - Organophosphorus Compounds/blood/chemistry/isolation & purification MH - Organothiophosphorus Compounds/*blood/chemistry/isolation & purification MH - Pesticides/*blood/chemistry/isolation & purification MH - Reproducibility of Results MH - Solid Phase Microextraction MH - Solvents/chemistry MH - Tandem Mass Spectrometry EDAT- 2018/01/27 06:00 MHDA- 2018/10/16 06:00 CRDT- 2018/01/27 06:00 PHST- 2017/10/26 00:00 [received] PHST- 2018/01/27 06:00 [pubmed] PHST- 2018/10/16 06:00 [medline] PHST- 2018/01/27 06:00 [entrez] AID - 4823130 [pii] AID - 10.1093/jat/bky004 [doi] PST - ppublish SO - J Anal Toxicol. 2018 Jun 1;42(5):321-329. doi: 10.1093/jat/bky004.