建立了同时测定肉制品中16种β-激动剂、6种头孢菌素类、6种青霉素类、3种氟喹诺酮类和2种糖肽类药物的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。样品经酶解后，以0.1%甲酸-乙腈（体积分数）提取，分散固相萃取净化，串联质谱ESI正、负模式电离，多反应监测（MRM）模式检测，以保留时间和子离子丰度比定性，外标法定量。结果表明，33种目标物在1.0～300 μg/L范围内线性关系良好，相关系数均大于0.996，β-激动剂和氟喹诺酮类药物的方法检出限（LOD，S/N=3）为0.5 μg/kg，其他目标物的LOD为3.0 μg/kg；加标水平为2.0~100 μg/kg时（n=6），平均回收率为74.9%~112%，相对标准偏差为2.2%~10.8%。方法准确、灵敏，适用于肉制品中β-激动剂、头孢菌素类、青霉素类、氟喹诺酮类和糖肽类等药物残留的高通量测定。

A high-throughput method was established for simultaneous determination of 33 β-agonists, six cephalosporins, six penicillins, three fluoroquinolones, and two glycopeptides in meat products by dispersive solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After enzymolysis treatment, the sample was extracted with 0.1% formic acid-acetonitrile (volume fraction), and purified with dispersive solid phase extraction. The resultant sample was analyzed by positive and negative electrospray ionization (ESI+/-) tandem mass spectrometry under multiple reaction monitoring (MRM) mode. The qualitative analysis was performed using retention time and ion abundance ratio, and the quantitative analysis was performed using external standard method. The results showed that the 33 target compounds displayed a good linearity in the concentration range of 1.0~300 μg/L, with correlation coefficients larger than 0.996. The limits of detection (LOD, S/N=3) were 0.5 μg/kg for β-agonists and fluoroquinolones and 3 μg/kg for the others. At spiked levels of 2.0~100 μg/kg, the average recoveries were in the range of 74.9~112%, and the RSDs ranged from 2.2% to 10.8%. The developed method is accurate, sensitive, and suitable for the high-throughput quantitative and qualitative analysis of β-agonist, cephalosporin, penicillin, fluoroquinolone, and glycopeptide multi-residues in meat products.

国家科技部港澳台科技合作专项基金资助（2013DFH30070）