UPLC-MS/MS法测定动物源性食品中4个四环素类药物和10个β受体激动剂类药物残留

目的：建立同时测定动物源性食品中4个四环素类药物和10个β受体激动剂类药物残留的新型超高效液相色谱-串联质谱方法。 方法：样品用三氯乙酸-乙腈提取并去除蛋白质，然后用Waters Acquity UPLC BEH C₁₈色谱柱（100 mm×2.1 mm，1.7 μm）分离，以0.05%甲酸水溶液和甲醇为流动相进行梯度洗脱（0~10.0 min，3.0%A→90.0%A；10.0~10.1 min，90.0%A→3.0%A；10.1~13.0 min，3.0%A），将待测药物分为多个时间段进行MRM扫描，四环素采用外标法定量，β受体激动剂类药物采用内标法定量。 结果：土霉素、金霉素、四环素及强力霉素在5.0~100.0 ng·mL^-1范围内呈良好的线性关系，相关系数（r）均大于0.990；检出限为2.0 ng·mL^-1，定量限为5.0 ng·mL^-1，10种β受体激动剂在1.0~50.0 ng·mL^-1范围内呈良好的线性关系，相关系数（r）均大于0.990；检出限为0.5 ng·mL^-1，定量限为1.0 ng·mL^-1。 结论：本研究前处理方法简单快捷，质谱采用多时间段MRM扫描方法，灵敏度显著提高，能够高效、灵敏地同时检测动物源性食品中的四环素类和β受体激动剂类药物。

Objective: To establish a method for the determination of 4 tetracyclines and 10β-agonist residues in animal products by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods: The animal-derived food was extracted with trichloroacetic acid and acetonitrile,and then separated on a Waters Acquity UPLC BEH C₁₈ column (100 mm×2.1 mm,1.7 μm).The mobile phase was 0.05% formic acid in water-methanol for gradient elution(0-10.0 min,3.0%A→90.0%A;10.0-10.1 min,90.0%A→3.0%A;10.1-13.0 min,3.0%A).4 tetracyclines and 10β-agonist residues were detected with MRM mode at multi-period. External standard method was employed for analyzing tetracyclines and internal standard method for β-agonist residues. Results: Under these conditions,the linear range for tetracyclines was 5.0-100.0 ng·mL^-1,the linear correlation coefficient was above 0.99,the limit of detection was 2.0 ng·mL^-1,and the limit of quantification was 5.0 ng·mL^-1. The linear range for β-agonist was 1.0-50.0 ng·mL^-1,the linear correlation coefficient was above 0.99,the limit of detection was 0.5 ng·mL^-1,and the limit of quantification was 1.0 ng·mL^-1. Conclusion: The established method is simple and sensitive,which can be used for the determination of tetracycline and β-agonist residues in animal-derived food.