PMID- 23831000 OWN - NLM STAT- MEDLINE DCOM- 20131022 LR - 20130716 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1302 DP - 2013 Aug 9 TI - Ultrasound-assisted dispersive liquid-liquid microextraction plus simultaneous silylation for rapid determination of salicylate and benzophenone-type ultraviolet filters in aqueous samples. PG - 20-7 LID - S0021-9673(13)00912-6 [pii] LID - 10.1016/j.chroma.2013.06.017 [doi] AB - A rapid procedure, using minimal amounts of solvent, for the reliable determination of five salicylate and benzophenone-type ultraviolet (UV) filters: ethylhexyl salicylate (EHS), 3,3,5-trimethyl-cyclohexyl salicylate (HMS), 2-hydroxy-4-methoxybenzophenone (BP-3), 2,4-dihydroxy-benzophenone (BP-1) and 2,2'-dihydroxy-4-methoxybenzophenone (BP-8), in aqueous samples is described. The method involves an ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) plus simultaneous silylation prior to their determination by gas chromatography-mass spectrometry (GC-MS). The parameters affecting the extraction and derivatization efficiency of the target UV filters from aqueous samples were systematically investigated and the conditions optimized. The optimal silylation and extraction conditions involved the rapid injection of a mixture of 750muL of acetone (as a dispersant), 15muL of tetrachloroethylene (as an extractant), and 20muL of BSTFA (as a derivatizing agent) into a 10-mL volume of aqueous samples (pH 7.0) containing 0.5g of sodium chloride in a glass tube with a conical bottom. After ultrasonication for 2.0min and centrifugation at 5000rpm (10min), the sedimented phase 5.0muL was directly introduced into the GC-MS. The limits of quantitation (LOQs) were less than 6ng/L. The precision for these analytes, as indicated by the relative standard deviations (RSDs), was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 74 and 92%. The method was then applied to environmental aqueous samples, using a standard addition method, showing the occurrence of BP-3 in samples of both river water and municipal wastewater treatment plant (MWTP) effluents. CI - Copyright (c) 2013 Elsevier B.V. All rights reserved. FAU - Wu, Jen-Wen AU - Wu JW AD - Department of Chemistry, National Central University, Chung-Li 320, Taiwan. FAU - Chen, Hsin-Chang AU - Chen HC FAU - Ding, Wang-Hsien AU - Ding WH LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20130618 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Benzophenones) RN - 0 (Salicylates) SB - IM MH - Benzophenones/*analysis MH - Filtration/methods MH - Liquid Phase Microextraction/*methods MH - Molecular Structure MH - Salicylates/*analysis OTO - NOTNLM OT - GC-MS OT - Organic UV filters OT - Simultaneous silylation OT - Ultrasound-assisted dispersive liquid-liquid microextraction OT - Water sample analysis EDAT- 2013/07/09 06:00 MHDA- 2013/10/23 06:00 CRDT- 2013/07/09 06:00 PHST- 2013/04/10 00:00 [received] PHST- 2013/06/10 00:00 [revised] PHST- 2013/06/11 00:00 [accepted] PHST- 2013/07/09 06:00 [entrez] PHST- 2013/07/09 06:00 [pubmed] PHST- 2013/10/23 06:00 [medline] AID - S0021-9673(13)00912-6 [pii] AID - 10.1016/j.chroma.2013.06.017 [doi] PST - ppublish SO - J Chromatogr A. 2013 Aug 9;1302:20-7. doi: 10.1016/j.chroma.2013.06.017. Epub 2013 Jun 18.