超高效液相色谱-四极杆/飞行时间质谱法快速筛查苹果中的螺虫乙酯及其代谢物

Rapid screening of spirotetramat and its metabolites in apples by ultra performance liquid chromatography with ultra resolution quadrupole time of flight mass spectrometry

目的建立超高效液相色谱-四极杆/飞行时间质谱法快速筛查苹果中的螺虫乙酯及其代谢物的分析方法。方法样品用乙腈和水提取后,盐析分层离心,经十八烷基键合硅胶(C18)和石墨化碳黑(graphitizing of carbon black,GCB)固相吸附剂净化后,采用电喷雾离子源和大气压化学离子源复合源和正离子扫描方式进行数据采集。结果 3种化合物标准曲线在0.5~250μg/L范围内呈良好线性关系,相关系数r大于0.9993,平均回收率为85.8%~99.2%,方法检出限为1.0~1.5μg/kg,方法定量限为3.0~5.0μg/kg,相对标准偏差为4.05%~6.20%。结论该方法高效快速、回收率高、灵敏度高、重现性好,可用于实际快速筛查苹果中的螺虫乙酯及其代谢物。

Objective To establish a method for rapid screening of spirotetramat and its metabolites in apples by ultra performance liquid chromatography-high resolution quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS). Methods Samples were extracted by acetonitrile and water, then salted out and centrifugated, and finally purified by solid phase extractant C18 and GCB. Data were detected with electron spray ionization (ESI) and atmospheric pressure chemical ion (APCI) composite sources in a positive ion mode. Results The calibration curves of 3 kinds of spirotetramat and its metabolites exhibited good linearities at the concentrations of 0.5?250 μg/L, and correlation coefficients (r) were greater than 0.9993. The average recoveries of 3 spike levels were 85.8%?99.2%, while the limits of detection and the limits of quantitation were 1.0?1.5 μg/kg and 3.0?5.0 μg/kg, respectively. The relative standard deviations (RSDs) were 4.05%?6.20%. Conclusion This method is efficient and rapid, with high recovery, high sensitivity and good reproducibility, which is suitable for rapid screening of spirotetramat and its metabolites in apples.