高效液相色谱-串联质谱法测定加工肉制品中莱克多巴胺及克伦特罗的含量

Determination of Ractopamine and Clenbuterol in Processed Meats by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱串联质谱测定加工肉制品中莱克多巴胺和克伦特罗的方法。采用阳离子交换色谱柱(SCX)分离目标化合物,改进了前处理方法,采用PXC固相萃取柱净化,并对洗脱溶液和高效液相色谱串联质谱的各参数进行优化。高效液相色谱流动相流速为0.4 mL/min,进样量为10μL,柱温为40℃。样品均质后加入30μLβ-盐酸葡萄糖醛苷酶-芳基硫酸酯酶,并经0.02 mol/L乙酸铵溶液(pH 5.2)提取,离心,过固相萃取柱净化。两种目标化合物在0.1～100μg/L范围内线性关系良好,检出限和定量下限分别不超过0.04μg/kg和0.15μg/kg。样品平均加标回收率为72%～98%,RSD低于8.5%。结果表明,此方法适于加工肉制品中莱克多巴胺和克伦特罗的测定。

A high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS） method was developed for the simultaneous determination of ractopamine and clenbuterol in processed meats.A new cation exchange chromatographic column was utilized to separate target compounds and an improved pre-treatment method was uesed in this study.The eluent solution types and chromatographic parameters were optimized.The optimal conditions were as follows： using a flow rate of 0.4 mL·min-1,a injection volume of 10 μL and a column temperature of 40 ℃.The homogenized samples were extracted with 0.02 mol·L-1 ammonium acetate（pH 5.2）,hydrolyzed with 30 μL β-glucuronidase/arylsulfatase,centrifuged,and cleaned through solid phase extraction column.The calibration curves showed good linearities for two target compounds in the range of 0.1-100 μg·L-1.The limits of detection and quantitation of two target compounds were not more than 0.04 μg/kg and 0.15 μg/kg,respectively.The spiked recoveries for the processed meats ranged from 72% to 98% with RSDs less than 8.5%.This proposed method was simple and sensitive,and was suitable for the quantification of ractopamine and clenbuterol in processed meats.