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目的:采用液相色谱串接质谱联用法对肉食品中残留的低浓度克仑特罗进行确证分析。方法:样品匀浆处理后,酸化去除蛋白,经液液萃取和MCX 3cc固相萃取柱两步纯化,以流动相为10 mmol/L的p H 3.5甲酸铵和乙腈为流动相,梯度洗脱,采用Eclipse C18(1.8μm,4.6×100 mm)色谱柱分离,电喷雾离子源,正离子多反应监测模式扫描分析检测。结果:D9-克仑特罗为内标,克仑特罗的线性范围为0.01~0.2μg/kg,相关系数(R2)大于0.99,检出限为0.005μg/kg,3个不同水平的加标回收率为78.8%~114.8%,相对标准偏差不大于10%。结论:该方法具有操作简单、灵敏度高、重现性好等特点,可以完成肉食品样品中痕量克仑特罗的确证分析。
OBJECTIVE: To confirm the low concentrations of clenbuterol residues in meat products by liquid chromatography tandem mass spectrometry. Methods: After the samples were homogenized, the proteins were removed by acidification and purified by liquid-liquid extraction and MCX 3cc SPE cartridges. The mobile phase consisted of p H 3.5 ammonium formate with 10 mmol / L mobile phase and acetonitrile as mobile phase. , Using Eclipse C18 (1.8μm, 4.6 × 100mm) column separation, electrospray ionization source, positive ion multi-reaction monitoring mode scanning analysis and detection. Results: The linear range of Clenbuterol was 0.01-0.2 μg / kg, the correlation coefficient (R2) was greater than 0.99, and the limit of detection was 0.005 μg / kg with three levels of D9-clenbuterol as internal standard Standard recovery was 78.8% ~ 114.8%, the relative standard deviation of not more than 10%. Conclusion: This method has the characteristics of simple operation, high sensitivity and good reproducibility, which can be used to confirm the confirmation of trace Clenbuterol in meat food samples.