超高效液相色谱串联质谱法测定蔬菜中31种抗生素

Simultaneous determination of 31 kinds of antibiotics in vegetables by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱串联质谱法  蔬菜  抗生素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  vegetables  antibiotics

中文摘要:

      目的 建立超高效液相色谱串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定蔬菜中31种抗生素药物的分析方法。方法 样品经Na2EDTA-Mcllvaine缓冲盐和1%甲酸-乙腈(V/V)提取, 无水硫酸钠及氯化钠脱水盐析, C18粉末净化, 以乙腈-5 mmol/L乙酸铵溶液为流动相进行梯度洗脱, 采用正离子扫描, 多反应监测(multiple reaction monitoring, MRM)模式, 使31种目标化合物在C18色谱柱上分离, 外标法定量。结果 31种目标化合物在2.0~200 ng/mL范围内线性关系良好, 相关系数均大于0.99, 方法检出限为0.5~2.0 μg/kg, 定量限为1.5~6.0 μg/kg。各种目标化合物在3个添加水平(8、20和50 μg/kg)下的回收率为76.6%~116.3%, 相对标准偏差(relative standard deviation, RSD) (n＝6)为2.2%~6.4%。结论 该方法操作简单、净化效果好, 适用于蔬菜中抗生素的快速检测。

英文摘要:

      Objective To establish a method for the determination of 31 antibiotics in vegetables by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted with Na2EDTA-Mcllvaine buffer salt and 1% formic acid acetonitrile (V/V), salted out with anhydrous sodium sulfate andsodium chloride, and then purified by C18 powder. The 31 compounds were separated on a C18 column by the gradient elution using acetonitrile-5 mmol/L ammonium acetate as mobile phase, detected by positive mode in multiple reaction monitoring (MRM) mode, and finally quanitified by external standard method. Results The correlation coeffcients r2 of the 31 compounds were all above 0.99 in the mass concentration range from 2.0? 200 ng/mL. The limits of detection and the limits of quantification of the method were 0.5?2.0 μg/kg and 1.5? 6.0 μg/kg, respectively. The recoveries spiked at 3 levels (8, 20 and 50 μg/kg) in matrix ranged from 76.6% to 115.4%, with the relative standard deviations (RSDs) 2.2%-6.4% (n=6). Conclusion This method is easy to operate and with good purification effect, which is suitable for the rapid determination of the antibiotics in vegetables