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Published:Journal of Chromatographic Science, ISSN 0021-9665Volume 39, Number 10, October 2001, pp.

Preparation and Characterization of 3-(Aza-18-Crown-6) Propylsilyl Bonded Phase for Reversed-Phase Liquid Chromatography

Shi-Lu Da, Yu-Qi Feng, Hui-Ning Da, Yin-Han Gong, and Yuan-Wei Zhang

39, Number 5, May 2001, pp. 177-182

Analysis of Endosulfan and Its Metabolites in Human Serum Using Gas Chromatography–Tandem Mass Spectrometry
F.J. Arrebola[1], J.L. Martínez Vidal[1], and A. Fernández-Gutiérrez[2]
[1] Department of Analytical Chemistry, University of Almería, 04071 Almería, Spain
[2] Department of Analytical Chemistry, University of Granada, 18071 Granada, Spain

A new analytical method combining solid-phase extraction and gas chromatography–tandem mass spectrometry (GC–MS–MS) is proposed to determine the insecticide endosulfan as well as its metabolites endosulfan-ether, -lactone, and -sulfate in human serum. Most matrix interferences are avoided using a cleanup step included in the sample treatment and an instrumental technique such as GC–MS–MS, which presents a high sensitivity and selectivity. Recoveries of spiked compounds range between 94.8 and 100.4% and 93.4 and 99.7% at fortification levels of 10 and 30 ng/mL, respectively. The relative standard deviation is lower than 17.6% in all cases, and the limits of detection calculated range from 6 to 19 pg/mL. Serum samples of nine agricultural workers that spray endosulfan into greenhouses in Almería (Spain) and two nonoccupationally exposed people are analyzed, and endosulfan is found in all the samples studied.

 

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