Kaur Ramandeep, Mandal Kousik, Kumar Rajinder, Singh Balwinder
Punjab Agricultural University, Department of Entomology, Pesticide Residue Analysis Laboratory, Ludhiana-141004, Punjab, India.
J AOAC Int. 2015 Mar-Apr;98(2):464-71. doi: 10.5740/jaoacint.13-066.
An easy, simple, and efficient analytical method was validated for the determination of residues of fipronil and its metabolites in different vegetables comprising brinjal, cabbage, capsicum, cauliflower, okra, and tomato. The Quick, Easy, Cheap, Rugged and Safe method was used for the extraction and cleanup of fipronil and its metabolites on these vegetables. Final clear extracts of ethyl acetate were concentrated under vacuum and reconstituted into acetone, and residues were determined by GC/MS with an Rtx-5 capillary column. The retention times of desulfinyl, sulfide, fipronil, sulfone, and amide were 11.8, 15.8, 16.4, 19.7, and 24.1 min, respectively. The average recoveries obtained for fipronil and its metabolites at different spiking levels were determined to be above 85% in all samples. The repeatability and reproducibility in different matrixes ranged from 1.36 to 5.42 and 1.75 to 4.53%, respectively, for fipronil and its metabolites. The LOQ of this method was 0.01 mg/kg and LOD was 0.003 mg/kg.
验证了一种简便高效的分析方法，用于测定茄子、卷心菜、辣椒、花椰菜、秋葵和番茄等不同蔬菜中氟虫腈及其代谢物的残留量。采用快速、简便、廉价、耐用且安全（Quick, Easy, Cheap, Rugged and Safe，即QuEChERS）方法对这些蔬菜中的氟虫腈及其代谢物进行提取和净化。将最终得到的乙酸乙酯澄清提取物在真空下浓缩，再用丙酮复溶，然后使用Rtx - 5毛细管柱通过气相色谱 - 质谱联用仪（GC/MS）测定残留量。脱亚砜基、硫化物、氟虫腈、砜和酰胺的保留时间分别为11.8、15.8、16.4、19.7和24.1分钟。在所有样品中，不同加标水平下氟虫腈及其代谢物的平均回收率均高于85%。氟虫腈及其代谢物在不同基质中的重复性和再现性分别为1.36%至5.42%和1.75%至4.53%。该方法的定量限为0.01 mg/kg，检测限为0.003 mg/kg。
