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  • Title: Solid-phase extraction of phosphorous-containing amino acid herbicides from biological specimens with a zirconia-coated silica cartridge.
    Author: Watanabe D, Ohta H, Yamamuro T.
    Journal: J Chromatogr B Analyt Technol Biomed Life Sci; 2014 Oct 15; 969():69-76. PubMed ID: 25151332.
    Abstract:
    We report a rapid solid-phase extraction method for glyphosate (Glyp), glufosinate (Gluf), and bialaphos (Bial) using a zirconia-coated silica cartridge, which interacts specifically with phosphorous-containing amino acid herbicides (PAAHs). We extracted PAAHs from serum and urine samples. The PAAHs were derivatized with trimethyl orthoacetate-acetic acid and analyzed by ultra-performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS). The intra-day and inter-day accuracy was within ±13% RE, the intra-day and inter-day precision was less than 12% RSD, and the total recovery was more than 60% for Glyp and more than 80% for Gluf and Bial. The linearity ranges of the calibration curves of the serum samples were 0.2-10,000μg/mL for Glyp, 0.1-1000μg/L for Gluf, and 0.5-1000μg/L for Bial; and those of the urine samples were 0.4-20,000μg/L for Glyp, 0.2-2000μg/L for Gluf, and 0.1-2000μg/L for Bial. This range covers almost all the reported poisoning cases involving these compounds, from very mild to fatal cases. The present paper offers a universal cleanup method for PAAHs in serum and urine samples for clinical and forensic analysis.
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