超高效液相色谱-串联质谱法同时测定动物源性食品中46 种食源性兴奋剂残留量

建立一种同时测定动物源性食品中46 种食源性兴奋剂的超高效液相色谱-串联质谱分析方法。样品于37 ℃酶解16 h，乙腈提取、乙腈饱和正己烷脱脂后，上清液经C18和中性氧化铝混合分散固相萃取（QuEChERS法）净化后，采用Waters ACQUITY BEH C18色谱柱分离，以0.005%甲酸溶液-甲醇为流动相进行梯度洗脱，使用电喷雾正负离子模式同时扫描检测，外标法定量。结果表明：46 种食源性兴奋剂在相应质量浓度范围内线性关系良好，相关系数均大于0.998，检出限为0.05～1.0 μg/kg，定量限为0.1～2.0 μg/kg，方法回收率为76.0%～111.9%，相对标准偏差为2.3%～12.4%（n=6）。该方法简便快速，实用性强，可为食源性兴奋剂检测提供有效技术支撑。

Simultaneous Determination of 46 Foodborne Stimulant Drug Residues in Animal-derived Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

A method was developed for the simultaneous detection of 46 foodborne stimulant drug residues in animal-derived foods by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were enzymatically digested for 16 h at 37 ℃, extracted with acetonitrile, defatted with n-hexane saturated with acetonitrile, purified by dispersive solid phase extraction (DSPE) with octadecylsilane bonded silica (C18) and neutral alumina as adsorbents, and finally separated on a Waters ACQUITY BEH C18 column by gradient elution using a mixture of 0.005% formic acid and methanol as the mobile phase. The detection was operated using an electrospray ionization mass spectrometer in both the positive and negative ion modes, and quantitation was performed by the external standard method. The results showed that good linear relationships were obtained for all the analytes in the investigated concentration ranges with correlation coefficients more than 0.998. The limits of detection (LODs) were 0.05–1.0 μg/kg, and the limits of quantitation (LOQs) were 0.1–2.0 μg/kg. Average recoveries of the analytes in pork ranged from 76.0% to 111.9%, with relative standard deviations (RSDs) of 2.3%–12.4%. The developed method is simple, rapid and practical, and can provide effective technical support for the detection of foodborne stimulant drug residues.