title: Fast determination of paraquat in plasma and urine samples by solid-phase microextraction and gas chromatography-mass spectrometry.
abstract: 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 0.1-50μg/mL. The limits of detection (S/N=3) were 0.01μg/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.
authors: School of Pharmacy, China Medical University, Shenyang 110001, PR China.
authors: Lina
authors: L
authors: Gao
authors: School of Pharmacy, China Medical University, Shenyang 110001, PR China. Electronic address: liujunting8@163.com.
authors: Junting
authors: J
authors: Liu
authors: School of Pharmacy, China Medical University, Shenyang 110001, PR China.
authors: Chunyuan
authors: C
authors: Wang
authors: College of Basic Medical Science, China Medical University, Shenyang 110001, PR China.
authors: Guojie
authors: G
authors: Liu
authors: School of Pharmacy, China Medical University, Shenyang 110001, PR China.
authors: Xiaodong
authors: X
authors: Niu
authors: School of Pharmacy, China Medical University, Shenyang 110001, PR China.
authors: Cuixia
authors: C
authors: Shu
authors: School of Pharmacy, China Medical University, Shenyang 110001, PR China.
authors: Juan
authors: J
authors: Zhu
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D008297:Male; D008875:Middle Aged; D010269:Paraquat / Q000097:blood* / Q000737:chemistry / Q000652:urine*; D015203:Reproducibility of Results; D012965:Sodium Chloride; D052617:Solid Phase Microextraction / Q000295:instrumentation / Q000379:methods*; D013405:Suicide; D013696:Temperature
chemical_list: D012965:Sodium Chloride; D010269:Paraquat
keywords: GC–MS; Paraquat; Plasma and urine samples; SPME