PMID- 21035660 OWN - NLM STAT- MEDLINE DCOM- 20110310 LR - 20191210 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 83 IP - 1 DP - 2010 Nov 15 TI - Analysis of sediment-associated insecticides using ultrasound assisted microwave extraction and gas chromatography-mass spectrometry. PG - 171-7 LID - 10.1016/j.talanta.2010.09.002 [doi] AB - 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. CI - Copyright (c) 2010 Elsevier B.V. All rights reserved. FAU - Li, Huizhen AU - Li H AD - State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China. FAU - Wei, Yanli AU - Wei Y FAU - You, Jing AU - You J FAU - Lydy, Michael J AU - Lydy MJ LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Validation Study DEP - 20100915 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R RN - 0 (Insecticides) RN - 0 (Organophosphates) SB - IM MH - Equipment Design MH - Gas Chromatography-Mass Spectrometry/*methods MH - Geologic Sediments/*analysis MH - Insecticides/*isolation & purification MH - *Microwaves MH - Organophosphates/*isolation & purification MH - Sensitivity and Specificity MH - Solid Phase Extraction/*instrumentation/methods MH - Ultrasonics/instrumentation/methods EDAT- 2010/11/03 06:00 MHDA- 2011/03/11 06:00 CRDT- 2010/11/02 06:00 PHST- 2010/06/22 00:00 [received] PHST- 2010/08/31 00:00 [revised] PHST- 2010/09/03 00:00 [accepted] PHST- 2010/11/02 06:00 [entrez] PHST- 2010/11/03 06:00 [pubmed] PHST- 2011/03/11 06:00 [medline] AID - S0039-9140(10)00697-1 [pii] AID - 10.1016/j.talanta.2010.09.002 [doi] PST - ppublish SO - Talanta. 2010 Nov 15;83(1):171-7. doi: 10.1016/j.talanta.2010.09.002. Epub 2010 Sep 15.