School of Pharmacy, China Medical University, Shenyang 110001, PR China.
School of Pharmacy, China Medical University, Shenyang 110001, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jan 1;944:136-40. doi: 10.1016/j.jchromb.2013.10.028. Epub 2013 Nov 20.
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.
建立了一种以乙基对草快为内标，采用硼氢化钠-氯化镍（NaBH4-NiCl2）还原和固相微萃取（SPME）的全氢化物化产物，用于检测和定量生物样品中百草枯浓度的简单、灵敏、可靠的气相色谱-质谱法（GC-MS）。在最佳条件下，血浆和尿液样品中的回收率分别为 94.00-99.85%和 95.00-100.34%。观察到良好的样品净化效果，在 0.1-50μg/mL 范围内具有良好的线性关系（血浆样品 r=0.9982，尿液样品 r=0.9987）。血浆和尿液样品的检测限（S/N=3）均为 0.01μg/mL。日内精密度小于 8.43%、4.19%（n=3），日间精密度小于 10.90%、10.49%（n=5）。该方法成功应用于因摄入百草枯而死亡的受害者生物样品的分析。
