同位素稀释/超高效液相色谱-四极杆-飞行时间质谱法测定牛蛙中50种兽药残留

Determination of 50 kinds of veterinary drug residues in Rana catesbiana by isotope dilution/ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry

目的建立同位素稀释/超高效液相色谱-四极杆-飞行时间质谱法(ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry, UPLC-Q-TOF-MS)测定牛蛙中50种兽药残留的分析方法。方法 样品用0.2%甲酸乙腈提取,经快速滤过型净化(multi-plug filtration cleanup,m-PFC)固相萃取柱处理,采用Phenomenex Kinetex C_(18)色谱柱分离,以0.1%甲酸乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,目标物在正离子全信息串联质谱扫描方式(mass spectrometry, MS^(E))下检测,内标法定量。结果 50种兽药在各自的质量浓度范围内线性关系良好,相关系数大于0.995,检出限为0.5~1.0μg/kg,加标回收率为79.4%~112.1%,相对标准偏差为3.7%~13.1%。结论 该方法前处理简单、结果准确,适用于牛蛙中50种兽药残留的快速检测。

Objective To establish a method for rapid determination of 50 kinds of veterinary drug residues in Rana catesbiana by isotope dilution/ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS). Methods The samples were extracted with 0.2% formic acid acetonitrile, treated with multi-plug filtration cleanup(m-PFC) solid phase extraction column, separated with Phenomenex Kinetex C_(18)chromatographic column, gradient eluted with 0.1% formic acid-acetonitrile and 0.1% formic acid aqueous solution as mobile phase, and the target was detected under positive ion full information tandem mass spectrometry(MS^(E))scanning mode, and quantified by internal standard method. Results The 50 kinds of veterinary drugs had good linear relationship within their respective mass concentration range, the correlation coefficient was greater than 0.995,and the limits of detection were 0.5-1.0 μg/kg, the average spiked recoveries were 79.4%-112.1%, and the relative standard deviations were 3.7%-13.1%. Conclusion This method has simple pre-processing and accurate results,and is suitable for rapid determination of 50 kinds of veterinary drugs residues in Rana catesbiana.