测定和消解花生及土壤中的氟虫腈及其代谢物。
Determination and dissipation of fipronil and its metabolites in peanut and soil.
机构信息
†College of Science, China Agricultural University, Beijing 100193, China.
§Institute of Quality Standards and Testing Technology for Agro-Products, Xinjiang Academy of Agricultural Sciences, Xinjiang 830091, China.
出版信息
J Agric Food Chem. 2015 May 13;63(18):4435-43. doi: 10.1021/jf5054589. Epub 2015 Feb 20.
In this study, a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was established for the extraction and cleanup of fipronil and its three metabolites (fipronil solfone, sulfide, and desulfinyl) in peanut kernel, shell, straw, seedling, and soil samples, and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used for analysis. The average recoveries were 66-116% at the level of 0.001-0.1 mg/kg with the RSD <19%, and the limit of detection was 0.3 ng/g for all matrices. The dissipation experiment results demonstrated that fipronil dissipated more rapidly in peanut seedling than in soil, with half-lives of <1 day in peanut seedling and 32-57 days in soil depending on the soil pH. The final residues at harvest of peanut kernels were all below 0.02 mg/kg, whereas in peanut shell and straw, the total highest residues were 0.99 and 0.30 mg/kg, respectively. Fipronil-desulfinyl and fipronil-sulfone were the highest residue metabolites in peanut plant (seedling and straw) and soil samples, respectively.
本研究建立了一种改良的快速、简便、廉价、有效、耐用和安全（QuEChERS）方法，用于提取和净化花生仁、壳、秸秆、幼苗和土壤样品中的氟虫腈及其三种代谢物（氟虫腈砜、硫醚和脱磺酰基），并采用液相色谱-串联质谱（LC-MS/MS）进行分析。在 0.001-0.1 mg/kg 水平下，平均回收率为 66-116%，相对标准偏差（RSD）<19%，所有基质的检出限均为 0.3 ng/g。消解实验结果表明，氟虫腈在花生幼苗中的消解速度快于在土壤中的消解速度，在 pH 值不同的土壤中，半衰期分别为<1 天和 32-57 天。收获时花生仁中的最终残留均低于 0.02 mg/kg，而在花生壳和秸秆中，总最高残留分别为 0.99 和 0.30 mg/kg。在花生植株（幼苗和秸秆）和土壤样品中，氟虫腈脱磺酰基和氟虫腈硫醚是最高残留代谢物。
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