QuEChERS结合液相色谱串联质谱法同时测定鸡蛋中氟虫腈与氯霉素等7种农兽药残留

Simultaneous determination of fipronil, chloramphenicol and other 7 kinds of pesticide and veterinary drug residues in eggs by liquid chromatography tandem mass spectrometry with QuEChERS

中文关键词:  QuEChERS  高效液相色谱-串联质谱法  农兽药残留  鸡蛋

英文关键词:QuEChERS  high performance liquid chromatography-tandem mass spectrometry  pesticide and veterinary drug residues  egg

中文摘要:

      目的 建立液相色谱-串联质谱法测定鸡蛋中氟虫腈与氯霉素等7种农兽药残留的分析方法。方法 样品经乙腈提取, QuEChERS法进一步净化, 离心后取上清液用氮气吹至近干, 残渣用初始流动相溶解。用 5 mmol/L乙酸铵溶液和乙腈作为流动相进行梯度洗脱, Poroshell 120 EC-C18色谱柱进行色谱分离, 使用电子喷雾离子源(electron spray ionization, ESI-)和选择反应监测(selected reaction monitoring, SRM)模式测定, 初始流动相配制标准曲线, 外标法定量。结果 本方法在8 min内完成7种目标化合物的分离分析。7种农兽药在1~50 μg/L范围内具有较好的线性关系, 相关系数均r2大于0.996。回收率在82.7%~117.8%之间, 相对标准偏差小于9.9%(n=6)。结论 该方法样品前处理简单、效率高、灵敏、可靠、适用测定鸡蛋中氟虫腈与氯霉素等7种农兽药残留。

英文摘要:

      Objective To establish an analytical method for the determination of 7 kinds of pesticide and veterinary drug residues including fipronil, chloramphenicol, etc in eggs by liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with acetonitrile and purified for a further step using a Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method. After centrifugation, the supernatant was taken and evaporated with nitrogen until nearly dry, the residue was dissolved by the initial mobile phase. The purified liquid was separated by the Poroshell 120 EC-C18 chromatographic column with a gradient elution using 5 mmol/L ammonium acetate solution and acetonitrile as the mobile phase. The mass spectrometry was carried out by electrospray ion source (ESI-) and selective response monitoring (selected reaction monitoring, SRM) mode, The initial mobile phase prepared the standard curve and quantified by external standard method. Results This method completed the separation and analysis of seven kinds of target compounds in 8 minutes. There was agood linear relationship among the seven kinds of agricultural and veterinary drugs in the range of 150 μg/L (relative coefficient, r2≥0.996), the recovery was 82.7%117.8%, and the relative standard deviation was less than 9.9%(n=6). Conclusion The method is simple, efficient, sensitive, reliable and can meet the requirement for simultaneous determination of fipronil, chloramphenicol and other 7 kinds of pesticide and veterinary drug residues in eggs.