Ultrasound-assisted dispersive liquid-liquid microextraction plus simultaneous silylation for rapid determination of salicylate and benzophenone-type ultraviolet filters in aqueous samples

Jen Wen Wu, Hsin Chang Chen, Wang Hsien Ding

研究成果: 雜誌貢獻期刊論文同行評審

71 引文 斯高帕斯(Scopus)

摘要

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 750 μL of acetone (as a dispersant), 15 μL of tetrachloroethylene (as an extractant), and 20 μL of BSTFA (as a derivatizing agent) into a 10-mL volume of aqueous samples (pH 7.0) containing 0.5. g of sodium chloride in a glass tube with a conical bottom. After ultrasonication for 2.0. min and centrifugation at 5000. rpm (10. min), the sedimented phase 5.0 μL was directly introduced into the GC-MS. The limits of quantitation (LOQs) were less than 6. ng/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.

原文???core.languages.en_GB???
頁(從 - 到)20-27
頁數8
期刊Journal of Chromatography A
1302
DOIs
出版狀態已出版 - 9 8月 2013

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