IDAEA., C.S.I.C., Environmental Chemistry Department, Jordi Girona 18-26, 08034 Barcelona, Spain.
J Chromatogr A. 2010 Apr 9;1217(15):2248-53. doi: 10.1016/j.chroma.2010.02.018. Epub 2010 Feb 16.
A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values < or =3-25% (n=5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were > or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1).
提出了一种简单、高效、环保的分析方法，用于在气相色谱-负化学电离质谱（GC-NCI-MS）分析之前从水样中提取和预浓缩拟除虫菊酯。本工作选择了 14 种拟除虫菊酯：联苯菊酯、氯氟氰菊酯、高效氯氟氰菊酯、顺式氯氰菊酯、溴氰菊酯、乙氰菊酯、氰戊菊酯、氯菊酯、氟胺氰菊酯、氯菊酯、苯醚菊酯、溴氰菊酯、四氟菊酯和三氟氯氰菊酯。该方法基于超声辅助乳化萃取（UAEE）在水介质中萃取水不混溶的溶剂。在 UAEE 技术中，氯仿被用作萃取溶剂。当用 20 mL 等分纯水溶液萃取添加拟除虫菊酯标准品的水样时，定量提取了目标分析物，实现了 200 的富集因子。该方法还用于自来水和河水样品的评估。方法检测限（MDL）范围为 0.03-35.8ng/L，相对标准偏差（RSD）值<或=3-25%（n=5）。采用所提出的方法获得的校准曲线的估算系数>或=0.998。回收率值在 45-106%范围内，表明该方法用于分析水样中的拟除虫菊酯具有良好的稳健性。该方法应用于河水样品的分析。在检测到的浓度范围内，顺式氯氰菊酯的浓度范围为 4.94-30.5ng/L。
