超高效液相色谱-串联质谱法测定动物源性食品中的磺胺增效剂

建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）测定多种基质（鸡肉、鱼肉、鸡肝、鸡蛋和牛奶）中三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶的分析方法。样品用甲酸-乙腈（1：9，v/v）溶液提取，正己烷除脂净化，Acquity UPLC BEH C18柱（50 mm×2.1 mm，1.7 μm）分离，以甲醇和5 mmol/L醋酸铵（含0.1%（v/v）甲酸）作为流动相进行梯度洗脱，电喷雾正离子（ESI⁺）模式电离，多反应监测（MRM）模式检测。考察了3种提取溶液的提取效率，优化了净化条件和浓缩条件，并对流动相、柱温和固相萃取柱进行了优化。结果表明：三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶在1.25~30.0 μg/L范围内线性关系良好（r≥0.99）。方法的定量限（S/N=10）为5.0 μg/kg，在5.0、10.0、20.0 μg/kg的添加浓度的回收率为61.2%~108.5%，相对标准偏差（RSD，n=6）为1.1%~9.8%。该方法快速、灵敏、准确，适合于多种基质中磺胺增效剂的测定。

Determination of sulfonamide potentiators in animal origin foods by ultra performance liquid chromatography-tandem mass spectrometry

A method for the determination of sulfonamide potentiators, trimethoprim (TMP), diaveridine (DVD) and ormetoprin (OMP), in different animal origin food matrices (including chicken muscle, fish muscle, chicken liver, egg and milk) has been developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted by formic acid-acetonitrile (1:9, v/v), cleaned-up by hexane, separated on an Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution. The determination was carried out with electrospray ion source under the positive mode and multiple reaction monitoring (MRM) mode. The extraction recoveries of three extraction solvents were observed. The purification condition and concentration condition were optimized. In addition, the mobile phase, column temperature and solid phase extraction column were studied. The calibration curves showed a good linearity in the range of 1.25-30.0 μg/L, and the correlation coefficients (r) were higher than 0.99. The limits of quantification (LOQ, S/N=10) of the three potentiators were 5.0 μg/kg. At the spiked levels of 5.0, 10.0 and 20.0 μg/kg, the recoveries of the three potentiators were ranged from 61.2% to 108.5%, and the relative standard deviations (RSD, n=6) ranged from 1.1% to 9.8%. The results indicate that the method is simple, rapid, sensitive and suitable for the qualitative and quantitative analysis of the three potentiators in multiple matrices.