Combination of Modified QuEChERS and Disposable Polyethylene Pipet Assisted DLLME Based on Low Density Solvent Extraction for Rapid and Sensitive Determination of Fipronil and Its Metabolites in Eggs by GC-MS
Combination of Modified QuEChERS and Disposable Polyethylene Pipet Assisted DLLME Based on Low Density Solvent Extraction for Rapid and Sensitive Determination of Fipronil and Its Metabolites in Eggs by GC-MS
复制标题
改进的 QuEChERS 与基于低密度溶剂萃取的一次性聚乙烯移液管辅助 DLLME 相结合，通过 GC-MS 快速灵敏地测定鸡蛋中的氟虫腈及其代谢物
DOI：
10.1007/s12161-020-01948-4
复制
发表时间：
2021
影响因子：
2.9
通讯作者：
Yu-Qi Feng
中科院分区：
文献类型：
--
作者：
Qin Zhao;Yi-Lian Zhou;Shi-Wen Yue;Yu-Jiao Lou;Yu-Qi Feng
本研究将改进的QuEChERS方法与一次性聚乙烯吸管辅助DLLME（DPP-DLLME）相结合，建立了一种分离富集鸡蛋中氟虫腈及其代谢物的新方法。DPP-DLLME采用低密度溶剂作为萃取剂，并在廉价的一次性聚乙烯移液管中进行，该移液管具有开放且狭窄的顶部。相分离后，萃取剂漂浮在水溶液上，并在移液管的窄颈中浓缩，其可直接由微量注射器抽取用于仪器分析。建立了鸡蛋中氟虫腈及其代谢物的气相色谱-质谱联用分析方法。线性范围为0.5-200 ng/g，相关系数R2> 0.9967。在鸡蛋中的加标回收率为89.3-103.8%，日内RSD小于13.6%，日间RSD小于17.5%。鸡蛋中四种目标分析物（非泼罗尼酰、非泼罗尼硫化物、非泼罗尼、非泼罗尼砜）的定量限在0.2-0.3 ng/g范围内，与先前报道的方法相当或更好。将建立的QuEChERS-DPP-DLLME方法成功应用于市售不同品牌鸡蛋样品中氟虫腈及其代谢物的检测。
In the present study, a new method for separation and enrichment of fipronil and its metabolites in eggs was proposed by combining a modified QuEChERS procedure with a disposable polyethylene pipet assisted DLLME (DPP-DLLME). The DPP-DLLME employed low density solvent as extractant and was conducted in a cheap, disposable polyethylene pipet with an open and narrow tip upside. After phase separation, the extractant was floating on the aqueous solution and concentrated in the narrow neck of the pipet, which can be directly withdrawn by a microsyringe for instrument analysis. By coupling with GC-MS detection, a new method for analysis of fipronil and its metabolites in eggs was established. The linearity range was 0.5–200 ng/g with correlation coefficientR2higher than 0.9967. The recoveries in spiked egg samples were in the range of 89.3–103.8% with the RSDs less than 13.6% (intra-day) and 17.5% (inter-day). The limits of quantification for the four target analytes (fipronil desulfinyl, fipronil sulfide, fipronil, fipronil sulfone) in eggs were in the range of 0.2–0.3 ng/g, which was comparable or better to the previously reported methods. Finally, the established QuEChERS-DPP-DLLME method was successfully applied to detect fipronil and its metabolites in several egg samples with different brands from local market.