PMID- 24558843 OWN - NLM STAT- MEDLINE DCOM- 20150708 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 31 IP - 11 DP - 2013 Nov TI - [Solvent demulsification-dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with gas chromatography-mass spectrometry for simultaneous determination of organochlorine pesticides in aqueous samples]. PG - 1076-80 AB - A novel method for simultaneous determination of eight organochlorine pesticides in solidification of floating organic drop coupled with gas chromatography-mass spectrometry (GC-MS) was established. A mixture of extractant (n-hexadecane) and dispersive agent (acetone) at the ratio of 1/5 (v/v) was injected into aqueous sample to form an emulsion and an extraction process was accomplished. The demulsifier (750 microL acetone) was then injected to break up the emulsion. The two phases were separated quickly without centrifugation. After being solidified in an ice-bath, the upper layer (n-hexadecane) was transferred into an Eppendorf tube and analyzed by GC-MS after melted at room temperature. Factors affecting extraction efficiency such as the type and volume of extractant, dispersive agent and demulsifier, also ionic strength and pH value of extraction system were studied. Under the optimized conditions, the working curve of the proposed method provided a good linearity in the range of 0.025-2.00 microg/L (r = 0.999 5-0.999 9). The detection limits of the organochlorine pesticides calculated by Hubaux-Vos method were 0.012-0.024 microg/L and the relative standard deviations (RSDs) ranged from 3.15% to 4.53%. The enrichment factors (EF) were 96-101. When the method was applied to the determination of farmland water, the average spiked recoveries were 96.77%-102.93% with the relative standard deviations of 2.68%-4.86%. The proposed method is sensitive and fast. It also has the advantage of little organic solvent consumption so that it is friendly to environment and suitable for batch analysis of organochlorine pesticides in aqueous samples. Meanwhile, it provides technical and methodological support for achieving the automation of sample pretreatment. FAU - Wang, Yu AU - Wang Y AD - West China School of Public Health, Sichuan University, Key Laboratory of Food Safety Risk Assessment and Monitoring of Sichuan Province, Chengdu 610041, China. FAU - Zhu, Chenghua AU - Zhu C AD - West China School of Public Health, Sichuan University, Key Laboratory of Food Safety Risk Assessment and Monitoring of Sichuan Province, Chengdu 610041, China. FAU - Zou, Xiaoli AU - Zou X AD - West China School of Public Health, Sichuan University, Key Laboratory of Food Safety Risk Assessment and Monitoring of Sichuan Province, Chengdu 610041, China. FAU - Huang, Lizhi AU - Huang L AD - West China School of Public Health, Sichuan University, Key Laboratory of Food Safety Risk Assessment and Monitoring of Sichuan Province, Chengdu 610041, China. FAU - Yan, Dong AU - Yan D AD - West China School of Public Health, Sichuan University, Key Laboratory of Food Safety Risk Assessment and Monitoring of Sichuan Province, Chengdu 610041, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Emulsions) RN - 0 (Hydrocarbons, Chlorinated) RN - 0 (Pesticide Residues) RN - 0 (Solvents) RN - 0 (Water Pollutants, Chemical) RN - 059QF0KO0R (Water) SB - IM MH - Emulsions MH - *Gas Chromatography-Mass Spectrometry MH - Hydrocarbons, Chlorinated/*analysis MH - *Liquid Phase Microextraction MH - Pesticide Residues/*analysis MH - Solvents MH - Water MH - Water Pollutants, Chemical/*analysis EDAT- 2014/02/25 06:00 MHDA- 2015/07/15 06:00 CRDT- 2014/02/25 06:00 PHST- 2014/02/25 06:00 [entrez] PHST- 2014/02/25 06:00 [pubmed] PHST- 2015/07/15 06:00 [medline] AID - 10.3724/sp.j.1123.2013.06008 [doi] PST - ppublish SO - Se Pu. 2013 Nov;31(11):1076-80. doi: 10.3724/sp.j.1123.2013.06008.