超高效液相色谱-串联质谱法测定牛肉中的阿托品

Determination of Atropine in Beef by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱法测定牛肉中阿托品残留量的分析方法。样品用0.1mol/L磷酸二氢钾缓冲溶液-乙腈(4∶1)提取,采用AgilentZorbaxEclipsePlusC18柱(4.6mm×50mm,2.7μm)为分离柱,以乙腈和0.1%甲酸水作为流动相,梯度洗脱。在电喷雾正离子模式下(ESI+),用多重反应监测(MRM)模式进行检测,基质匹配外标法定量。在优化的实验条件下,阿托品的检出限为0.5μg/kg,定量限为1.5μg/kg,线性范围为0.10~5.0ng/mL,相关系数r≥0.999。在1.0、5.0和10μg/kg这3个加标水平下,阿托品的平均回收率为89.5%~95.2%,相对标准偏差(RSD6)为2.07%~5.03%。该方法简单、灵敏度高、结果准确可靠,可用于牛肉中阿托品残留量的测定。

A method was developed for determination of Atropine in beef using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Samples were extracted with 0.1 mol/L phosphate buffer solution:Acetonitrile(4∶1).The target analyte was separated on an Agilent Zorbax Eclipse Plus C18 column(4.6 mm×50 mm,2.7 μm) with gradient elution using acetonitrile and water with 0.1%(volume ration) formic acid as mobile phases.Atropine was determined by multiple reaction monitoring(MRM) mode with electrospray positive ion soure,and quantified by black matrix external standard.Under the optimal experimental conditions,LOD of Atropine was 0.5 μg/kg,and LOQ was 1.5 μg/kg.The method showed a good linearity of Atropine in the range of 0.10~5.0 ng/mL with correlation coefficients more than 0.999.The average recoveries for samples spiked at three levels(1.0,5.0 and 10 μg/kg) were ranged from 89.5% to 95.2%,and the relative standard deviations(RSD6) from 2.07% to 5.03%.This method was simple,sensitive,accurate and reliable,which could be applied to the detection of Atropine in beef.