PMID- 30987786 OWN - NLM STAT- MEDLINE DCOM- 20190628 LR - 20190628 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1599 DP - 2019 Aug 16 TI - In-situ derivatization and headspace solid-phase microextraction for gas chromatography-mass spectrometry analysis of alkyl methylphosphonic acids following solid-phase extraction using thin film. PG - 17-24 LID - S0021-9673(19)30364-4 [pii] LID - 10.1016/j.chroma.2019.04.010 [doi] AB - A headspace solid-phase microextraction (HS-SPME) method, involving solid-phase extraction and in-situ derivatization using polymeric thin film, was developed for the gas chromatography-mass spectrometry (GC-MS) analysis of the degradation products of nerve agents. The solid-phase extraction (SPE) was performed using poly([2-(Methacryloyloxy)ethyl]trimethylammonium chloride) film on a gold plate prepared via surface-initiated polymerization. The extracted analytes were directly derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) on the plate. Various parameters like fiber type, headspace time, temperature, and amount of BSTFA were optimized. Under the optimized conditions, the relative standard deviations (RSDs) were in the range 7.0-13.1% and the limits of detection (LODs) were measured to be between 10 and 20 pg mL(-1). The application of the developed method was tested using the 35th Organization for Prohibition of Chemical Weapons (OPCW) proficiency test sample. CI - Copyright (c) 2019 Elsevier B.V. All rights reserved. FAU - Kim, Hyunsuk AU - Kim H AD - Center for Cell-Encapsulation Research, Department of Chemistry, KAIST, Daejeon, 34141, South Korea; Chemical and Biological Defense Department, Agency for Defense Development, Daejeon, 34186, South Korea. FAU - Cho, Yungyeong AU - Cho Y AD - Chemical and Biological Defense Department, Agency for Defense Development, Daejeon, 34186, South Korea. FAU - Lee, Bong Soo AU - Lee BS AD - Center for Cell-Encapsulation Research, Department of Chemistry, KAIST, Daejeon, 34141, South Korea. Electronic address: leebongsoo@kaist.ac.kr. FAU - Choi, Insung S AU - Choi IS AD - Center for Cell-Encapsulation Research, Department of Chemistry, KAIST, Daejeon, 34141, South Korea. Electronic address: ischoi@kaist.ac.kr. LA - eng PT - Journal Article DEP - 20190408 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Nerve Agents) RN - 0 (Organophosphorus Compounds) RN - 0 (Polymers) RN - 329W4YM10Z (methylphosphonic acid) SB - IM MH - Chemistry Techniques, Analytical/*methods MH - *Gas Chromatography-Mass Spectrometry MH - Limit of Detection MH - Nerve Agents/chemistry/isolation & purification MH - Organophosphorus Compounds/*analysis/chemistry MH - Polymers/*chemistry MH - *Solid Phase Microextraction/instrumentation MH - Temperature OTO - NOTNLM OT - GC-MS OT - HS-SPME OT - In-situ derivative OT - Nerve agents OT - SI-ARGET ATRP OT - Solid-Phase extraction EDAT- 2019/04/17 06:00 MHDA- 2019/06/30 06:00 CRDT- 2019/04/17 06:00 PHST- 2019/01/23 00:00 [received] PHST- 2019/04/04 00:00 [revised] PHST- 2019/04/06 00:00 [accepted] PHST- 2019/04/17 06:00 [pubmed] PHST- 2019/06/30 06:00 [medline] PHST- 2019/04/17 06:00 [entrez] AID - S0021-9673(19)30364-4 [pii] AID - 10.1016/j.chroma.2019.04.010 [doi] PST - ppublish SO - J Chromatogr A. 2019 Aug 16;1599:17-24. doi: 10.1016/j.chroma.2019.04.010. Epub 2019 Apr 8.