MethodsX (Jan 2023)

A simultaneous, high-throughput and sensitive method for analysing 13 neonicotinoids and metabolites in urine using a liquid chromatography–tandem mass spectrometry

  • Yukiko Nishihama, PhD,
  • Shoji F. Nakayama, MD, PhD,
  • Tomohiko Isobe, PhD

Journal volume & issue
Vol. 10
p. 102129

Abstract

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A simultaneous, high-throughput and sensitive method for analysing nine neonicotinoid pesticides (NEOs) and four metabolites (NEOms) in urine using a liquid chromatography-tandem mass spectrometry (LC–MSMS) was developed. The method detection limit (MDL) and lowest concentration minimum reporting limit (LCMRL) of the nine NEOs were 0.0013–0.048 ng/ml and 0.0050–0.17 ng/ml, respectively. The MDL and LCMRL of the four NEOms were 0.0052–0.52 ng/ml and 0.011–1.6 ng/ml, respectively. Intermediate precision for the nine NEOs and four NEOms was 7.5–12.5% and 7.4–10.9%, respectively. Accuracy for the nine NEOs and four NEOms was 3.83–5.60% and 3.01–29.2%, respectively. The developed method was applied to analyse urine samples collected from participants of a large-scale birth cohort study, namely, the Japan Environment and Children's Study (JECS). • The NEO and NEOm concentrations in 100 µl urine samples were analysed using a highly sensitive LC–MSMS. • Automated solid phase extraction in a 96-well plate was utilised to achieve high-throughput analysis. • Intermediate precision and accuracy were less than 12.5% and 94.8–99.1%, respectively.

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