超高效液相色谱—串联质谱法测定原料奶中苯并咪唑类药物

Determination of Benzimidazoles Residue in Raw Milk Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了超高效液相色谱—串联四级杆质谱法测定原料奶中苯并咪唑类药物残留量的检测方法。原料奶经乙酸乙酯提取,MCX固相萃取柱净化,用UPLC-MS/MS进行检测。色谱条件为:色谱柱为ACQUITYUPLCTMBEHC18柱(2.1 mm×100 mm,1.7μm);流动相为:乙腈-0.1%甲酸水溶液,梯度洗脱,流速为0.3 mL/min。采用ESI正离子模式,多反应监测(MRM)模式检测,外标法定量。本方法检测测苯并咪唑类药物残留的检测限为0.5μg/kg,定量限为1.0μg/kg。

A method for determination of benzimidazoles residue in raw milk was developed using ultra performance liquid chromatography - tandem mass spectrometry （ UPLC - MS/MS）. Ethyl acetate was used to extract the target analyte from raw milk, extraction was degreased and cleaned up with Waters Oasis MCX solid phase extraction （SPE） column for UPLC - MS/MS. The liquid chromatography separation was carried on Cls column （2.1 mm × 100 mm i. d. ,1.7 μm） with acetonitrile and water（added 0.1% formic acid） as mobile phase at a flow rate of 0.3mL/min. The mass spectrometry was performed in multiple reaction monitoring（MRM） mode. The limits of detection （LOD） of the method were 0.5 μg/kg and the limits of quantification （LOQ） were 1.0μg/kg. The method has good repeatability and high sensitivity , and can be applied for the determination of benzimidazoles in raw milk.