气相色谱法和高效液相色谱-串联质谱法测定 鸡蛋中氟虫腈及代谢物残留

Determination of fipronil and its metabolites residues in chicken egg by gas chromatography and high performance liquid chromatography-tandem mass spectrometry

中文关键词:  鸡蛋  氟虫腈及其代谢物  气相色谱法  高效液相色谱-串联质谱法

英文关键词:chicken egg  fipronil and its metabolite  gas chromatography  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立适用于鸡蛋中氟虫腈及其代谢物(氟虫腈砜、氟虫腈硫醚和氟甲腈)残留的电子捕获检测器-气相色谱法和高效液相色谱-串联质谱检测方法。方法 通过QuEChERS提取盐包(CEN EN-15662)用乙腈提取目标化合物, 借助固相萃取(PRiME HLB)作为净化手段, 采用气相和液相质谱进行监测。结果 气相色谱法和高效液相色谱-串联质谱法中4种分析物的定性限(limit of detection, LOD)分别为0.1 μg/kg和0.02 μg/kg; 定量限(limit of quantification, LOQ)分别为0.5 μg/kg和0.1 μg/kg, 在0.1~10.0 μg/L和0.1~5.0 μg/L范围内线性关系良好, 相关系数r2均大于0.999。在2.5, 5和10 μg/kg 3种加标浓度下, 平均回收率分别为80.8%~103%和87.4%~101%, 相对标准偏差(relative standard deviation, RSD, n=6)分别为0.84%~5.62%和0.87%~4.40%。 结论 该方法步骤简便、可靠、稳定, 适合于蛋类中氟虫腈及其代谢物残留的痕量分析。

英文摘要:

      Objective To establish two methods for determination of fipronil and its metabolites residues in chicken egg by gas chromatography and high performance liquid chromatography-tandem mass spectrometry. Methods Egg sample was diluted with water and extracted with acetronitrile by QuEChERS extraction tube (CEN EN-15662). The extracts were purified by the PRiME HLB solid phase extraction cartridge prior to analysis. Results The limits of detection (LODs) and the limits of quantification (LOQs) of fipronil and its metabolites in egg were 0.1 and 0.5 μg/kg by gas chromatography method, respectively, and were 0.02 and 0.1 μg/kg by high performance liquid chromatography-tandem mass spectrometry, respectively. Good linearity was obtained when the concentrations of the two methods were within 0.1-10 μg/L and 0.1-5 μg/kg. The correlation coefficients (r2) were greater than 0.999. The average recoveries of gas chromatography and high performance liquid chromatography-tandem mass spectrometry were within 80.8%~103% and 87.4%-101% at the spiked concentrations of 2.5, 5 and 10 μg/kg, with the relative standard deviations (RSDs, n=6) of 0.84%-5.62% and 0.87%-4.40%. Conclusion The methods are simple, sensitive and reliable, which are suitable for trace analysis of fipronil and its metabolite residues in eggs.