PMID- 20638501 OWN - NLM STAT- MEDLINE DCOM- 20101202 LR - 20141120 IS - 1873-4324 (Electronic) IS - 0003-2670 (Linking) VI - 674 IP - 1 DP - 2010 Jul 26 TI - Simultaneous determination of phoxim and its photo-transformation metabolite residues in eggs using liquid chromatography coupled with electrospray ionization tandem mass spectrometry. PG - 64-70 LID - 10.1016/j.aca.2010.06.016 [doi] AB - The principal objective of this study was to develop an appropriate, sensitive, and selective method for the simultaneous quantitative determination of phoxim and its photo-transformation product, O,O-diethyl alpha-cyanobenzylideneamino-thiophosphonate (DCTP) in both chicken and quail eggs. Eggs (1 g) were blended with anhydrous magnesium sulfate (1 g) for sample pretreatment and extracted with acetonitrile. The extracts were then further purified with SPE silica gel tubes deactivated with trimethylamine. Residues were analyzed via a reversed phase-liquid chromatography-tandem mass spectrometry (RP-LC-MS/MS) in positive-ion electrospray ionization (ESI) mode. Tebufenozide was utilized as an internal standard for the quantification of phoxim and its metabolite residues. The identification and quantification of analytes were based on ion transitions monitored by multiple reaction monitoring (MRM). LC-MS/MS analysis was performed from 0.02 to 1 mg kg(-1) and correlation coefficients (r(2)) ranging from 0.998 to 0.999 were obtained for both analytes in blank egg extracts. The relative standard deviations (RSDs) of intra- and inter-day variations ranged from 2.1% to 6.7% and from 2.8% to 6.4% for phoxim and DCTP in chicken and quail eggs. At all levels of fortification (0.02, 0.05, and 0.125 mg kg(-1)), the recoveries fell within a range of 81.3% to 93.6% for phoxim and 83.3% to 90.1% for DCTP. The matrix effect was <2%, due to the partial dilution of the sample. Decision limits (CCalpha) and detection capabilities (CCbeta) were in the range of 0.0005-0.0044 and 0.0054-0.0224 mg kg(-1), respectively. The method was evaluated further by analyzing real samples purchased from markets. All chicken and quail egg samples were free from residues of the target compounds. CI - Copyright 2010 Elsevier B.V. All rights reserved. FAU - Lee, Jung Han AU - Lee JH AD - Department of Chemistry and Research Institute of Life Science, Gyeongsang National University, Jinju 660-701, Republic of Korea. FAU - Park, Semin AU - Park S FAU - Jeong, Won Young AU - Jeong WY FAU - Park, Hyung Jin AU - Park HJ FAU - Kim, Hae Gyeong AU - Kim HG FAU - Lee, Soo-Jung AU - Lee SJ FAU - Shim, Jae-Han AU - Shim JH FAU - Kim, Soo Taek AU - Kim ST FAU - Abd El-Aty, A M AU - Abd El-Aty AM FAU - Im, Moo Hyeog AU - Im MH FAU - Choi, Ok Ja AU - Choi OJ FAU - Shin, Sung Chul AU - Shin SC LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20100623 PL - Netherlands TA - Anal Chim Acta JT - Analytica chimica acta JID - 0370534 RN - 0 (Organothiophosphorus Compounds) RN - 0 (Pesticide Residues) RN - 6F5V775VPO (phoxim) SB - IM MH - Chromatography, Reverse-Phase MH - Eggs/*analysis MH - Organothiophosphorus Compounds/*analysis/metabolism MH - Pesticide Residues/*analysis/metabolism MH - Spectrometry, Mass, Electrospray Ionization MH - Tandem Mass Spectrometry EDAT- 2010/07/20 06:00 MHDA- 2010/12/14 06:00 CRDT- 2010/07/20 06:00 PHST- 2010/04/15 00:00 [received] PHST- 2010/06/13 00:00 [revised] PHST- 2010/06/14 00:00 [accepted] PHST- 2010/07/20 06:00 [entrez] PHST- 2010/07/20 06:00 [pubmed] PHST- 2010/12/14 06:00 [medline] AID - S0003-2670(10)00754-3 [pii] AID - 10.1016/j.aca.2010.06.016 [doi] PST - ppublish SO - Anal Chim Acta. 2010 Jul 26;674(1):64-70. doi: 10.1016/j.aca.2010.06.016. Epub 2010 Jun 23.