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Development and validation of a novel UFLC-MS/MS method for the detection of biomarkers of organophosphate pesticide metabolites in urine.
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  • Sukesh Narayan Sinha,
  • Dileshwar Kumar,
  • Ramakrishna Ungarala,
  • * KVasudev
Sukesh Narayan Sinha
National Institute of Nutrition

Corresponding Author:[email protected]

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Dileshwar Kumar
Osmania University Faculty of Science
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Ramakrishna Ungarala
National Institute of Nutrition
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* KVasudev
National Institute of Nutrition
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Abstract

Rationale: Occupational or environmental exposure to organophosphate pesticides widely used worldwide can lead to significant health problems. Monitoring the levels of dialkyl phosphates (DAP) metabolites in human urine is a common biomarker for assessing such exposure. In this study developing a new screening method using ultra-fast liquid chromatography coupled with tandem mass spectrometry (UFLC-MS/MS) to detect six DAP metabolites in human urine. Methods: Three different compound extraction methods, namely QuEChERS, lyophilization, and liquid extraction, were compared in this study. The performance of each method was evaluated based on the recovery rate. The liquid extraction method provided better results and required only 20 minutes for analysis. The recovery rate, repeatability and reproducibility were determined to assess the method reliability. Additionally, the limits of detection and limits of quantitation were established to determine the lowest concentrations at which the method could reliably detect and quantify the DAP metabolites. Results: The liquid extraction method demonstrated superior performance compared to the other extraction methods, with a high recovery rate ranging from 93% to 112%. The repeatability (RSD) values ranged from 0.62% to 5.46%, indicating good precision within the same laboratory. The reproducibility (RSD) values ranged from 0.80% to 11.33%, indicating acceptable variability between laboratories or analysts. The LOD values ranged from 0.0201 ng/mL to 0.0697 ng/mL, and the LOQ values ranged from 0.0609 ng/mL to 0.2112 ng/mL, indicating the method’s sensitivity. Conclusions: The developed UFLC-MS/MS method are sensitive, and selective technique for detecting six DAP metabolites of organophosphate pesticides in human urine. The method successfully analysed 150 urine samples from farmers and non-farmers, demonstrating its applicability in biomonitoring studies. This method is particularly advantageous as it requires fewer samples, chemicals, materials, and time, making it an efficient and reliable approach for assessing occupational or environmental exposure to organophosphate pesticides.