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Phosphorus-specific determination of glyphosate, glufosinate, and their hydrolysis products in biological samples by liquid chromatography–inductively coupled plasma–mass spectrometry

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Anion exchange liquid chromatography (LC) with inductively coupled plasma–mass spectrometry (ICP–MS) was used for simultaneous determination of glyphosate and glufosinate (phosphonic and amino acid group-containing herbicides; PAAHs) and their hydrolysis products, aminomethylphosphonic acid (AMPA) and 3-methylphosphinicoacetic acid (MPPA), in biological samples. The target compounds were separated using an anion exchange resin column and gradient elution with sodium carbonate and sodium hydroxide system. The chromatographic eluates were passed through a membrane suppressor system and monitored by phosphorus-specific detection at m/z 31. PAAHs and their hydrolysis products were baseline separated from each other within 40 min of elution time, and phosphoric acid did not interfere with detection. The detection limits in serum samples were 0.1–0.7 µg/ml; those in urine samples, 0.2–1.6 µg/ml for the four compounds. The spiked recoveries for the four compounds were over 91 % in serum and urine samples. The detection of the compounds was not subject to interference from sample matrix components. The present method would be useful for toxicological analysis of PAAHs and their products in actual forensic practice. To our knowledge, this is the first trial to establish an LC–ICP–MS method for analysis of PAAHs and their products in biological samples .

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Correspondence to Yuko Kazui.

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Kazui, Y., Seto, Y. & Inoue, H. Phosphorus-specific determination of glyphosate, glufosinate, and their hydrolysis products in biological samples by liquid chromatography–inductively coupled plasma–mass spectrometry. Forensic Toxicol 32, 317–322 (2014).

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  • Glyphosate
  • Glufosinate
  • Aminomethylphosphonic acid (AMPA)
  • 3-Methylphosphonicoacetic acid (MPPA)
  • Biological samples