通过型固相萃取净化-超高效液相色谱-串联质谱法检测鸡肉中23种磺胺类药物残留

建立了通过型固相萃取净化超高效液相色谱-串联质谱法同时检测鸡肉中23种磺胺类药物残留的分析方法。鸡肉样品经80%乙腈溶液（含0.2%甲酸）提取，Oasis PRiME HLB固相萃取柱进行净化，用Waters Acquity UPLC CSH C18色谱柱（100 mm×2.1 mm，1.7 μm）分离，以甲醇和0.1%甲酸溶液为流动相梯度洗脱，电喷雾源正离子扫描及依赖保留时间的多反应监测模式下（Scheduled MRM）检测，外标法定量。结果表明:23种磺胺类药物在线性范围0.2~20 ng/mL上有良好的线性关系，相关系数均大于0.9996；检出限为0.1~2.0 μg/kg，定量限为0.25~5.0 μg/kg；在1.0、2.0、5.0 μg/kg三个加标水平上平均回收率为66.12%~99.83%，相对标准偏差（RSD，n=6）为0.72%~10.36%；该方法操作简单、灵敏度高、重现性好，适用于鸡肉中多种磺胺类药物残留的检测。

Determination of 23 Sulfonamide Drugs Residues in Chicken by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for simultaneous determination of 23 sulfonamide drugs residues in chicken. The samples were extracted by 80% acetonitrile solution (containing 0.2% formic acid) and the extracts were purified on Oasis PRiME HLB solid-phase extraction column. The 23 sulfonamide drugs were analyzed by Waters Acquity UPLC CSH C18 column (100 mm×2.1 mm, 1.7 μm) using methanol and 0.1% formic acid as the mobile phases, electrospray source positive ion scanning and retention time-dependent multiple reaction monitoring mode (Scheduled MRM) detection, external standard method for quantification. The results showed that there was a good linear relationship between 23 sulfonamide drugs in the linear range of 0.2~20 ng/mL, with the correlation coefficients all greater than 0.9996. The detection limits were 0.1~2.0 μg/kg, and the quantification limits were 0.25~5.0 μg/kg. The average recovery rates were 66.12%~99.83% and the relative standard deviations (RSD, n=6) form 0.72% to 10.36% at the three standard levels of 1.0, 2.0 and 5.0 μg/kg. The method is simple, sensitive and reproducible. The method is successfully used for accurate and quantitative measurement of multiple sulfanilamide drugs residues in chicken.