4.8 Article

Dimethoxytriadinylation LC-MS/MS of Novichok A-Series Degradation Products in Human Urine

Journal

ANALYTICAL CHEMISTRY
Volume 94, Issue 11, Pages 4658-4665

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/acs.analchem.1c04634

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Funding

  1. JSPS KAKENHI [JP 19K16364]

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This study developed a screening method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to detect and identify Novichok A-series degradation products and alkyl methylphosphonic acids in urine samples. The method utilized a suitable derivatization reagent and achieved the detection and stability of the target compounds. The newly developed method was successfully applied to analyze urine samples from a proficiency test.
Novichok A-series compounds, novel nerve agents, pose an increasing threat to citizens worldwide; however, no analytical methods have been reported for detecting their hydrolysis products. Herein, a screening method was developed to detect and identify Novichok A-series degradation products (hydrolysates of A230, A232, A234, A262, and one related compound) and alkyl methylphosphonic acids (RMPAs, conventional nerve agent hydrolysates) using liquid chromatography-tandem mass spectrometry (LC-MS/MS). We identified a suitable derivatization reagent, 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (DMTMM), and optimized the reaction conditions. The derivatized esters of Novichok A-series degradation products were stable and easily detected. We used this derivatization to achieve the first analytical method for Novichok hydrolysis products in urine (0.40-4.0 ng/mL). The detection limits of the RMPAs (0.1-0.4 ng/mL) were comparable to those presented in previous reports involving pentafluorobenzylation or direct LC-MS/MS. The applicability of the newly developed method was evaluated by analyzing urine samples from the OPCW Fifth Biomedical Proficiency Test.

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