Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Original Papers
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
Takeshi SAITOHiromichi AOKIAkira NAMERAHiroshi OIKAWAShota MIYAZAKIAkihiro NAKAMOTOSadaki INOKUCHI
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JOURNAL FREE ACCESS

2011 Volume 27 Issue 10 Pages 999

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Abstract

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-C18 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 μg/ml, respectively, for organophosphates, 0.1 and 0.5 μg/ml, respectively for GLUF and GLYP. The method had linear calibration curves ranging from 0.1 to 25.0 μg/ml for organophosphates and 0.5 – 100.0 μg/ml for GLUF, and GLYP. The validated method was successfully applied to a clinical GLYP poisoning case.

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© 2011 by The Japan Society for Analytical Chemistry
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