超低温冷冻-QuEChERS-气相色谱-负化学源-质谱联用法测定糟蛋中氟虫腈及其代谢物

Determination of fipronil and its metabolites in wine cued egg by ultra-low temperature cryo-QuEChERS combined with gas chromatography- negative chemical source-mass spectrometry

中文关键词:  氟虫腈及其代谢物  超低温冷冻  糟蛋  QuEChERS  负化学源  气相色谱-质谱联用法

英文关键词:fipronil and its metabolites  ultra-low temperature freezing  wine cued egg  QuEChERS  negative chemical source  gas chromatography-mass spectrometry

中文摘要:

      目的 建立气相色谱-负化学源-质谱联用法检测平湖糟蛋中氟虫腈及其代谢物的分析方法。方法 样品经乙腈提取后, 利用超低温冷冻去脂和QuEChERS分散固相萃取净化。采用负化学源(negative chemical ionization, NCI), 以选择离子监测(selected ion monitoring, SIM)模式对氟虫腈及其代谢物的定量离子和定性离子进行监测, 基质匹配标准曲线法定量。结果 氟虫腈及其代谢物在0.5~10 μg/L范围内呈良好的线性关系, 线性相关系数均大于0.999, 检出限在0.050~0.102 μg/kg范围内。样品添加浓度在2~10 μg/kg范围时, 其回收率为94.5%~117.9%, 相对标准偏差为2.05%~5.30%(n=6)。结论 本方法快速、简便、灵敏, 测定结果准确可靠, 满足糟蛋中氟虫腈及其代谢物残留量的测定。

英文摘要:

      Objective To establish a method for the determination of fipronil and its metabolites in Pinghu wine cued egg by gas chromatography-negative chemical source-mass spectrometry. Methods After extracted by acetonitrile, the samples were purified by ultra-low temperature freezing degreasing and QuEChERS dispersive solid phase extraction. The quantitative and qualitative ions of fipronil and its metabolites were monitored by negative chemical ionization (NCI) and selected ion monitoring (SIM), and quantified by matrix matching standard curve method. Results Fipronil and its metabolites showed a good linear relationship in the range of 0.5?10 μg/L, the linear correlation coefficients were all greater than 0.999, and the detection limits were in the range of 0.050? 0.102 μg/kg. The recoveries were 94.5%?117.9%, and the relative standard deviations were 2.05%?5.30% (n=6) in the range of 2?10 μg/kg. Conclusion This method is rapid, simple, sensitive, accurate and reliable for the determination of fipronil and its metabolites in wine cued egg.