Einsle T, Paschke H, Bruns K, Schrader S, Popp P, Moeder M
UFZ-Centre for Environmental Research Leipzig-Halle in the Helmholtz Association, Department of Analytical Chemistry, Permoserstrasse 15, D-04318 Leipzig, Germany.
J Chromatogr A. 2006 Aug 18;1124(1-2):196-204. doi: 10.1016/j.chroma.2006.06.093. Epub 2006 Jul 25.
Selected polycyclic musk compounds and drugs were extracted from water samples by membrane-assisted micro liquid-liquid extraction. The two-phase extraction system consisted of polyethylene membrane bags filled with an organic solvent. Chloroform proved to be most suited as acceptor phase to extract caffeine, Galaxolide, Tonalide, phenazone and carbamazepine from aqueous samples. The compounds were enriched from 50 mL sample into a volume of 500 microL of chloroform. Gas chromatography-mass spectrometry (GC-MS) was applied for analysis. The extraction procedure was optimised in regard to membrane material, extraction time and temperature. The evaluation of the entire analysis protocol found limits of detection that ranged from 20 to 200 ng/L. The linear range of calibration covered one magnitude with standard deviations between 4 and 12%. Method comparison with standard analysis techniques such as solid-phase extraction (SPE) combined with GC-MS as well as LC-MS-MS confirmed this method as an easy and reliable protocol, even for the monitoring of matrix-loaded wastewater. The analysis of real samples established the feasibility of the technique.
通过膜辅助微液-液萃取从水样中提取选定的多环麝香化合物和药物。两相萃取系统由填充有机溶剂的聚乙烯膜袋组成。事实证明，氯仿作为接受相最适合从水样中萃取咖啡因、佳乐麝香、吐纳麝香、非那宗和卡马西平。这些化合物从50 mL样品中富集到500 μL氯仿中。采用气相色谱-质谱联用仪（GC-MS）进行分析。在膜材料、萃取时间和温度方面对萃取程序进行了优化。对整个分析方案的评估发现，检测限在20至200 ng/L之间。校准的线性范围涵盖一个数量级，标准偏差在4%至12%之间。与标准分析技术如固相萃取（SPE）结合GC-MS以及液相色谱-串联质谱联用仪（LC-MS-MS）的方法比较证实，即使对于监测含有大量基质的废水，该方法也是一种简单可靠的方案。实际样品分析证实了该技术的可行性。
