2018年深圳市售蔬菜和鸡蛋中氟虫腈及其代谢物的检测分析

Detection and analysis of fipronil and its metabolites in vegetables and eggs sold in Shenzhen in 2018

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

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  fipronil and metabolites  eggs  vegetables

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定蔬菜和鸡蛋中氟虫腈及其代谢物(氟甲腈、氟虫腈砜和氟虫腈亚砜), 并对深圳市售的蔬菜和鸡蛋中氟虫腈及其代谢物残留状况进行抽样检测。方法 采用QuEChERS前处理方法, 以C18色谱柱为分离柱, 以乙腈和10 mmol甲酸+6 mmol甲酸铵水溶液为流动相进行梯度洗脱, 用超高效液相色谱-串联质谱(ultra performance liquid chromatography-mass spectrometry/mass spectrometry, UPLC-MS/MS), 电喷雾电离(electrospray ionization, ESI), 多反应监测(multiple reaction monitoring, MRM)模式检测, 外标法同时定量测定氟虫腈及其代谢物。结果 方法的线性范围为0.1~2.0 μg/L, 线性相关系数均大于0.9994, 检出限0.0005 mg/kg, 定量限0.001 mg/kg; 蔬菜中3个水平的平均加标回收率88.0%~101.2%, 相对标准偏差(relative standard deviation, RSD)均小于8.5%; 鸡蛋中3个水平的平均加标回收率86.1%~104.8%, 相对标准偏差(RSD)均小于9.2%。结论 该方法具有操作简单、干扰少、快速、准确可靠等特点, 可适用于蔬菜鸡蛋中氟虫腈及其代谢物的检测。

英文摘要:

      Objective To establish a method for determination of fipronil and metabolites (fipronil-desulfinyl, fipronil sulfone and fipronil sulfide) in vegetables and eggs, and fipronil and metabolites in vegetables and eggs from Shenzhen market were detected. Methods Using QuEChERS pretreatment method, the separation was performed on a C18 column with the gradient elution of acetonitrile and 10 mmol formic acid and 6 mmol ammonium formate in aqueous solution. The fipronil and metabolites in vegetables and eggs were detected by ultra performance liquid chromatography-mass spectrometry/mass spectrometry (UPLC-MS/MS) with eletrospray ionization (ESI) in mode of multiple reaction monitoring. Quantification was performed by external standard calibration. Results The calibration curves of fipronil and metabolites showed good linearity in range of 0.1-2.0 μg/L, with correlation coefficient in range of 0.9994-1.000. The limit of detection of the method was 0.0005 mg/kg. The limit of quantitative of the method was 0.001 mg/kg. The recoveries of 3 spiking levels in vegetables were from 88.0% to 101.2%, with the relative standard deviations (RSDs) of all less than 8.5%. The recoveries of 3 spiking levels in eggs were from 86.1% to 104.8%, with the RSDs of all less than 9.2%. Conclusion This method has the characteristics of simple operation, less interference, rapid, accurate and reliable, which can be applied to the detection of flurofenitrile and its metabolites in vegetable eggs.