Chemical Safety Division, Department of Agro-Food Safety and Crop Protection, National Institute of Agricultural Sciences, Rural Development Administration, Wanju, Republic of Korea.
Planning and Coordination Bureau, Rural Development Administration, Jeonju, Republic of Korea.
PLoS One. 2020 Oct 6;15(10):e0235526. doi: 10.1371/journal.pone.0235526. eCollection 2020.
Since broflanilide is a newly developed pesticide, analytical methods are required to determine the corresponding pesticide residues in diverse crops and foods. In this study, a pesticide residue analysis method was optimized for the detection and quantification of broflanilide and its two metabolites, DM-8007 and S(PFH-OH)-8007, in brown rice, soybean, apple, green pepper, mandarin, and kimchi cabbage. Residue samples were extracted from the produce using QuEChERS acetate and citrate buffering methods and were purified by dispersive solid-phase extraction (d-SPE) using six different adsorbent compositions with varying amounts of primary secondary amine (PSA), C18, and graphitized carbon black. All the sample preparation methods gave low-to-medium matrix effects, as confirmed by liquid chromatography-tandem mass spectrometry using standard solutions and matrix-matched standards. In particular, the use of the citrate buffering method, in combination with purification by d-SPE using 25 mg of PSA and a mixture of other adsorbents, consistently gave low matrix effects that in the range from -18.3 to 18.8%. Pesticide recoveries within the valid recovery range 70-120% were obtained both with and without d-SPE purification using 25 mg of PSA and other adsorbents. Thus, the developed residue analysis method is viable for the determination of broflanilide and its metabolites in various crops.
由于溴氟虫酰胺是一种新开发的农药，因此需要分析方法来确定不同作物和食品中相应的农药残留。本研究优化了一种用于检测和定量糙米、大豆、苹果、青椒、橘子和泡菜中溴氟虫酰胺及其两种代谢物 DM-8007 和 S(PFH-OH)-8007 的农药残留分析方法。采用 QuEChERS 乙酸盐和柠檬酸盐缓冲方法从农产品中提取残留样品，并用六种不同吸附剂组成的分散固相萃取（d-SPE）进行净化，吸附剂组成中含有不同量的初级/次级胺（PSA）、C18 和石墨化炭黑。所有的样品制备方法都得到了低到中等的基质效应，这通过使用标准溶液和基质匹配标准的液相色谱-串联质谱法得到了证实。特别是，使用柠檬酸盐缓冲方法，结合使用 25mg PSA 和其他吸附剂的混合物进行 d-SPE 净化，始终能得到低基质效应，范围在-18.3 到 18.8%之间。使用 25mg PSA 和其他吸附剂进行 d-SPE 净化和不进行 d-SPE 净化，都能在 70-120%的有效回收率范围内获得农药回收率。因此，所开发的残留分析方法可用于各种作物中溴氟虫酰胺及其代谢物的测定。
