State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China.
Talanta. 2010 Nov 15;83(1):171-7. doi: 10.1016/j.talanta.2010.09.002. Epub 2010 Sep 15.
An ultrasound assisted microwave extraction (UAME) method was developed to simultaneously extract five organophosphate (OP) and eight pyrethroid insecticides from sediment. The optimized UAME conditions were to use 100ml of a mixture of hexane and acetone (1:1, v/v) solution as the extraction solvents, and extraction time, microwave and ultrasonic power settings of 6 min, 100 W and 50 W, respectively. Extracts were cleaned using solid phase extraction and analyzed by gas chromatography-mass spectrometry in negative chemical ionization mode and quantification was based on matrix-matched standard solutions along with internal standard calibration. At the spiked concentrations of 1, 5 and 20 ng/g dry weight (dw), recoveries of OPs were 77.6-122%, 65.2-128% and 75.6-141% with relative standard deviations (RSDs) of 10.6-18.1%, 3.1-12.5% and 8.0-35.3%, respectively, while recoveries of pyrethroids were 78.0-101%, 76.4-104% and 71.0-99.5% with RSDs of 10.3-23.5%, 4.7-17.6% and 8.8-18.7%, respectively. Method detection limits ranged from 0.31 to 0.45 ng/g dw for the OP insecticides and from 0.27 to 0.70 ng/g dw for the pyrethroid insecticides. The newly developed UAME method was validated by comparing it to Soxhlet and sonication extraction methods. Better recoveries were achieved for most OPs by the novel UAME method, whereas there was no significant difference in recoveries for most of the pyrethroids. Finally, the UAME method was used to quantify the target insecticides in field-contaminated sediment samples which were collected in Guangzhou, China.
建立了超声辅助微波萃取（UAME）方法，用于同时从沉积物中提取五种有机磷（OP）和八种拟除虫菊酯杀虫剂。优化的 UAME 条件是使用 100ml 正己烷和丙酮（1:1，v/v）混合溶液作为萃取溶剂，萃取时间、微波和超声功率分别为 6min、100W 和 50W。萃取物通过固相萃取进行净化，并在负化学电离模式下通过气相色谱-质谱进行分析，定量基于基质匹配标准溶液和内标校准。在 1、5 和 20ng/g 干重（dw）的加标浓度下，OP 的回收率为 77.6-122%、65.2-128%和 75.6-141%，相对标准偏差（RSD）为 10.6-18.1%、3.1-12.5%和 8.0-35.3%，而拟除虫菊酯的回收率为 78.0-101%、76.4-104%和 71.0-99.5%，RSD 为 10.3-23.5%、4.7-17.6%和 8.8-18.7%。OP 类杀虫剂的方法检测限范围为 0.31-0.45ng/g dw，拟除虫菊酯的方法检测限范围为 0.27-0.70ng/g dw。通过与索氏提取和超声提取方法进行比较，验证了新开发的 UAME 方法的有效性。对于大多数 OP，新的 UAME 方法可获得更好的回收率，而对于大多数拟除虫菊酯，回收率没有显著差异。最后，使用 UAME 方法对中国广州采集的受污染沉积物现场样品中的目标杀虫剂进行定量。
