A novel extraction method for simultaneous determination of neonicotinoid insecticides and their metabolites in human urine

Analytical methods

Mingwei Gui¹  Tao Zhang¹  Shiming Song¹  Bo Zhang¹  Jiping Ouyang¹  Yuan He¹ 

[1] School of Environmental Science and Engineering, Sun Yat-Sen University, 135 Xingang West Street,Guangzhou 510275,China

DOI  :  10.1039/C9AY00288J

学科分类：分析化学

来源: Royal Society of Chemistry

【 摘 要 】

In this study, a novel method (i.e., liquid–liquid micro-extraction, LLME) coupled to liquid chromatography tandem mass spectrometry is proposed for the simultaneous determination of urinary levels of six neonicotinoid insecticides (NEOs), namely, imidacloprid, clothianidin, acetamiprid, thiacloprid, thiamethoxam, and dinotefuran, and four metabolites, including 1-methyl-3-(tetrahydro-3-furylmethyl) guanidine, 1-methyl-3-(tetrahydro-3-furylmethyl) urea, 5-hydroxy-imidacloprid, and N-demethyl-acetamiprid has been developed. Ethyl acetate was used as the extraction solvent, and the supernatant was concentrated and dissolved by methanol. The method was validated for repeatability, reproducibility, linearity, and percent recovery. Satisfactory recovery of the NEOs and their metabolites (71–107%) was observed with intraday relative standard deviations (RSDs, n = 3) of 2–11% and inter-day RSDs (n = 9) of 3–17%. Good linearity (R2 > 0.99) was obtained for all analytes. Limits of quantification and detection for all target analytes ranged from 0.01 ng mL−1 to 0.1 ng mL−1 and from 0.003 ng mL−1 to 0.03 ng mL−1, respectively. Trace levels of NEOs and their metabolites were found in human urine samples (mean: 0.06–1.99 ng mL−1). To the best of our knowledge, this study is the first to apply the proposed LLME method for simultaneous identification and quantification of NEOs and their metabolites in urine samples.

【 授权许可】

CC BY-NC