Applicability of cloud point extraction coupled with microwave-assisted back-extraction to the determination of organophosphorous pesticides in human urine by gas chromatography with flame photometry

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• 作者：GuiFang Jia ; ChunGuang Lv ; WenTao Zhu ; Jing Qiu ; XinQuan Wang ; ZhiQiang Zhou
• 关键词：Cloud point extraction ; Organophosphorous pesticides (OPPs) ; Microwave-assisted back-extraction ; Gas chromatography with flame photometry detection (GC-FPD) ; Human urine
• 刊名：Journal of Hazardous Materials
• 出版年：2008
• 出版时间：30 November 2008
• 年：2008
• 卷：159
• 期：2-3
• 页码：300-305
• 全文大小：359 K

文摘

A procedure for the determination of organophosphorous pesticides (OPPs) – phorate, diazinon, parathion-methyl, fenthion and quinalphos – in human urine was developed using the cloud point extraction of nonionic surfactant (Triton X-114) coupled with microwave-assisted back-extraction prior to gas chromatography with flame photometry detection (GC-FPD) analysis. The upper organic solution obtained from back-extraction was centrifugated simply for further cleanup for the sake of automatic injection. A preconcentration factor of 50 was obtained for these five OPPs extracted from only 10 mL of a sample. The limits of detection (LODs) were 0.07 ng mL⁻¹ for phorate, fenthion and quinalphos, 0.04 ng mL⁻¹ for diazinon and 0.08 ng mL⁻¹ for parathion-methyl. The limits of quantification (LOQs) were 0.21, 0.12, 0.24, 0.21 and 0.21 ng mL⁻¹, respectively. Accuracy of the method was evaluated by bias, which ranged from +6.85 to −14.68 % . Precision was also good; the relative standard deviations (R.S.D.s) were less than 9 % . The method showed to be potential for biological monitoring.