Fast determination of paraquat in plasma and urine samples by solid-phase microextraction and gas chromatography-mass spectrometry

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• 作者：Lina Gao ; Junting Liu ; Chunyuan Wang ; Guojie Liu ; Xiaodong Niu ; Cuixia Shu ; Juan Zhu
• 关键词：Paraquat ; Plasma and urine samples ; SPME ; GC&ndash ; MS
• 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
• 出版年：1 January, 2014
• 年：2014
• 卷：944
• 期：Complete
• 页码：136-140
• 全文大小：724 K

文摘

A simple, sensitive and reliable gas chromatographic-mass spectrometric method (GC-MS) for quantifying paraquat concentration in biological samples has been developed, using ethyl paraquat as an internal standard. The method involved the procedures of sodium borohydride-nickel chloride (NaBH₄-NiCl₂) reduction and solid-phase microextraction (SPME) of the perhydrogenated products. GC-MS was used to identify and quantify the analytes in selected ion monitoring (SIM) mode. Under the optimal conditions, recoveries in plasma and urine samples were 94.00-99.85% and 95.00-100.34%, respectively. Excellent sample clean-up was observed and good linearities (r = 0.9982 for plasma sample and 0.9987 for urine sample) were obtained in the range of 0.1-50 渭g/mL. The limits of detection (S/N = 3) were 0.01 渭g/mL in plasma and urine samples. The intra-day precision was less than 8.43%, 4.19% (n = 3), and inter-day precision was less than 10.90%, 10.49% (n = 5) for plasma and urine samples, respectively. This method was successfully applied to the analysis of the biological samples collected from a victim who died as a result of ingestion of paraquat.