Mix-mode TiO-C18 Monolith Spin Column Extraction and GC-MS for the Simultaneous Assay of Organophosphorus Compounds and Glufosinate, and Glyphosate in Human Serum and Urine
Mix-mode TiO-C18 Monolith Spin Column Extraction and GC-MS for the Simultaneous Assay of Organophosphorus Compounds and Glufosinate, and Glyphosate in Human Serum and Urine
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DOI：
10.2116/analsci.27.999
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发表时间：
2011-10-01
影响因子：
1.6
通讯作者：
Inokuchi, Sadaki
中科院分区：
文献类型：
--
作者：
Saito, Takeshi;Aoki, Hiromichi;Inokuchi, Sadaki
一种通过气相色谱-质谱 (GC-MS) 同步定量人血清和尿液中有机磷酸酯（杀螟松 (MEP)、马拉硫磷和酚妥特 (PAP)）、草铵膦 (GLUF) 和草甘膦 (GLYP) 的快速、特异且灵敏的方法已得到验证。使用混合模式 TiO-C-18 整体式旋转柱从血清和尿液中提取所有目标化合物以及内标。血清和尿液中有机磷的回收率为 12.7% 至 49.5%。血清和尿液中 GLUF 和 GLYP 的回收率为 1.9% 至 7.9%。内部和内部准确度和精密度（表示为相对标准偏差，%RSD）分别在 96.7 - 107.7% 和 4.0 - 13.8% 范围内。血清和尿液的检测限和定量限分别为：有机磷酸酯为 0.1 和 0.1 μg/ml，GLUF 和 GLYP 分别为 0.1 和 0.5 μg/ml。该方法的线性校准曲线范围为：有机磷酸酯为 0.1 至 25.0 μg/ml，GLUF 和 GLYP 为 0.5 - 100.0 μg/ml。经验证的方法已成功应用于临床 GLYP 中毒病例。
A rapid, specific, and sensitive method for the simultaneous quantitation of organophosphates (fenitrothion (MEP), malathion, and phenthoate (PAP)), glufosinate (GLUF), and glyphosate (GLYP) in human serum and urine by gas chromatography-mass spectrometry (GC-MS) has been validated. All of the targeted compounds together with the internal standard were extracted from the serum and urine using a mix-mode TiO-C-18 monolithic spin column. The recovery of organophosphates from serum and urine ranged from 12.7 to 49.5%. The recovery of GLUF and GLYP from serum and urine ranged from 1.9 to 7.9%. The intra- and inter-accuracy and precision (expressed as relative standard deviation, %RSD) were within 96.7 - 107.7% and 4.0 - 13.8%, respectively. The detection and quantitation limits for serum and urine were 0.1 and 0.1 mu g/ml, respectively, for organophosphates, 0.1 and 0.5 mu g/ml, respectively for GLUF and GLYP. The method had linear calibration curves ranging from 0.1 to 25.0 mu g/ml for organophosphates and 0.5 - 100.0 mu g/ml for GLUF, and GLYP. The validated method was successfully applied to a clinical GLYP poisoning case.