PMID- 18922539 OWN - NLM STAT- MEDLINE DCOM- 20090122 LR - 20191210 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1211 IP - 1-2 DP - 2008 Nov 21 TI - Speciation of butyltin compounds in environmental and biological samples using headspace single drop microextraction coupled with gas chromatography-inductively coupled plasma mass spectrometry. PG - 135-41 LID - 10.1016/j.chroma.2008.09.089 [doi] AB - A method based on headspace single drop microextraction (HS-SDME) in combination with gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS) was proposed for the speciation analysis of butyltin compounds in environmental and biological samples. The sodium tetraethylborate (NaBEt4) and sodium tetrahydroborate (NaBH4) were used as the derivatizing reagent for in situ derivatization of the butyltins. For the two derivatizations, the HS-SDME parameters such as organic solvent, drop volume, sample pH, stirring rate, temperature, extraction time and the ionic strength were examined systematically. The analytical performance including the linearity ranges, limits of detection (LODs) and reproducibilities of the two derivatizations were compared under the respective optimized conditions. Derivatization with NaBEt(4) proved to be more sensitive and robust than that with NaBH4, leading to the LODs of 1.4 ng/L for MBT, 1.8 ng/L for DBT and 0.8 ng/L for TBT. The reproducibilities, expressed as relative standard deviations (RSDs), were in the range of 1.1-5.3% (c=1 microg/L, n=3). With tripropyltin (TPrT) as internal standard, HS-SDME-GC-ICP-MS with NaBEt(4) derivatization was applied for the speciation analysis of butyltins in real seawater and shellfish samples. The butyltins found in the real-world samples are 31ng/L MBT, 79 ng/L DBT and 32 ng/L TBT for seawater, and 11.6-30.4 ng/g MBT, 11.8-8.9 ng/g DBT and 12.8-52.6 ng/g TBT for different shellfish samples. For validation, the developed method was also employed for the speciation analysis of butyltins in certified reference material (CRM) of PACS-2 sediment, and the determined values are in a good agreement with the certified values. The developed method is simple, rapid, sensitive, and cost-effective and provides an attractive alternative for butyltins speciation in biological and environmental samples with complex matrix. FAU - Xiao, Qin AU - Xiao Q AD - Department of Chemistry, Wuhan University, Wuhan 430072, China. FAU - Hu, Bin AU - Hu B FAU - He, Man AU - He M LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20081002 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Borates) RN - 0 (Borohydrides) RN - 0 (Organotin Compounds) RN - 0 (Solvents) RN - 15523-24-7 (sodium tetraethylborate) RN - 87L0B9CPPA (sodium borohydride) SB - IM MH - Animals MH - Borates/chemical synthesis MH - Borohydrides/chemical synthesis MH - Chemical Fractionation/*methods MH - Gas Chromatography-Mass Spectrometry/economics/methods MH - Hydrogen-Ion Concentration MH - Organotin Compounds/*analysis MH - Osmolar Concentration MH - Reference Standards MH - Reproducibility of Results MH - Seawater/*chemistry MH - Sensitivity and Specificity MH - Shellfish/*analysis MH - Solvents/chemistry MH - Temperature EDAT- 2008/10/17 09:00 MHDA- 2009/01/23 09:00 CRDT- 2008/10/17 09:00 PHST- 2008/08/08 00:00 [received] PHST- 2008/09/23 00:00 [revised] PHST- 2008/09/26 00:00 [accepted] PHST- 2008/10/17 09:00 [pubmed] PHST- 2009/01/23 09:00 [medline] PHST- 2008/10/17 09:00 [entrez] AID - S0021-9673(08)01683-X [pii] AID - 10.1016/j.chroma.2008.09.089 [doi] PST - ppublish SO - J Chromatogr A. 2008 Nov 21;1211(1-2):135-41. doi: 10.1016/j.chroma.2008.09.089. Epub 2008 Oct 2.