高效液相色谱-串联质谱法快速测定食物中毒样品中的百草枯和敌草快

Rapid determination of paraquat and diquat in food poisoning samples by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  食物中毒  百草枯  敌草快  尿液  血液

英文关键词:high performance liquid chromatography-tandem mass spectrometry  paraquat  diquat  foodstuff  urine  blood

中文摘要:

      目的 建立高效液相色谱-串联质谱法快速检测食物中毒事件中常见样品(如食品、血液及尿液等)中百草枯和敌草快的分析方法。方法 分别以乙酸乙酯为溶剂提取食品和尿液样品、以乙腈为溶剂提取血液样品中的百草枯和敌草快, 提取液氮吹浓缩至近干, 加入流动相复溶, 再经0.22 μm滤膜过滤。采用WATERS ACQUITY UPLC BEH Amide色谱柱分离, 以乙腈(A)-100 mmol/L甲酸铵溶液(含0.05%甲酸) (B)(60:40, V:V)为流动相等度洗脱, 多反应模式监测, 外标法定量。结果 百草枯和敌草快在2.0~100 μg/L质量浓度范围内线性关系良好, 相关系数为0.9971~0.9999。百草枯和敌草快的检出限(S/N=3)分别为1.0 μg/L和0.3 μg/L, 定量限(S/N=10)分别为3.0 μg/L和1.0 μg/L。加标水平为2.0、10.0、80.0 μg/L时, 百草枯和敌草快回收率分别为82.4%~98.4%和90.1%~103.5%, 相对标准偏差分别为0.8%~5.1%和1.0%~4.2%。结论 本方法建立的分析过程样品前处理简单、快速、准确, 适用于食品、血液和尿液中的百草枯和敌草快的同时测定。

英文摘要:

      Objective To establish a method for rapid determination of paraquat and diquat in related food poisoning samples such as food, blood and urine by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Food and urine samples were extracted with ethyl acetate and blood samples were extracted with acetonitrile. Paraquat and diquat were extracted with liquid nitrogen and blown to near-dry, then redissolved in mobile phase and filtered by 0.22 m filtration membrane. The samples were separated with WATERS ACQUITY UPLC BEH Amide column using acetonitrile (A)-100 mmol/L ammonium formate (containing 0.05% formic acid) (B) (60:40, V:V) as mobile phase for isocratic elution, monitored by multi-reaction mode, and quantified by external standard method. Results Paraquat and diquat had good linear relationships within the mass concentration range of 2.0?100 μg/L, and the correlation coefficients were 0.9971?0.9999. For paraquat and diquat, limits of detection (LOD) (S/N=3) were 1.0 μg/L and 0.3 μg/L, and limits of quantification (LOQ) (S/N=10) were 3.0 μg/L and 1.0 μg/L, respectively. When spiked with 3 concentration levels of 2.0, 10.0, and 80.0 μg/L, the recovery rates of paraquat and diquat were 82.4%?98.4% and 90.1%?103.5%, respectively, with relative standard deviations of 0.8%?5.1% and 1.0%?4.2%. Conclusion The analysis process established by this method is simple, fast and accurate, and is suitable for the simultaneous determination of paraquat and diquat in food, blood and urine.