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目的建立超高效液相色谱-电喷雾串联质谱法检测猪肉组织中克伦特罗、莱克多巴胺、沙丁胺醇和特布他林4种β-受体激动剂类药物残留。方法样品用β-盐酸葡萄糖醛苷酶酶解,经乙酸乙酯提取,经MCX固相萃取小柱净化,以Eclipse Plus C_(18)色谱柱(2.1 mm×50 mm,1.8μm)分离,以0.1%甲酸、2 mmol/L乙酸铵水溶液和0.1%甲酸乙腈溶液为流动相进行梯度洗脱。质谱分析以电喷雾为离子源,采用多反应监测,以正离子扫描模式进行检测。结果 4种β-受体激动剂类药物在0.5~50 ng/mL浓度范围内呈良好的线性关系,相关系数r~2≥0.9973,方法定量限为0.1μg/kg,平均回收率为65.5%~109.1%,相对标准偏差为6.6%~15.4%(n=6)。结论本方法具有定量限低、准确度高及稳定性好等特点,可以满足样品检测的要求。
OBJECTIVE To establish a method for the determination of four β-agonists in clenbuterol, ractopamine, salbutamol and terbutaline in pork by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry. Methods The samples were digested with β-HCG glucosidase, extracted with ethyl acetate, purified by MCX solid phase extraction cartridges and separated by Eclipse Plus C 18 column (2.1 mm × 50 mm, 1.8 μm) 0.1% formic acid, 2 mmol / L ammonium acetate aqueous solution and 0.1% formic acid in acetonitrile as the mobile phase. Mass spectrometry analysis using electrospray ionization as a source, using multiple reaction monitoring, positive ion scan mode detection. Results Four kinds of β-agonists showed a good linearity in the range of 0.5-50 ng / mL with a correlation coefficient of r ≥ 2.9999. The limit of quantification was 0.1 μg / kg and the average recovery was 65.5% ~ 109.1%, the relative standard deviation was 6.6% ~ 15.4% (n = 6). Conclusion The method has the advantages of low quantitative limit, high accuracy and good stability, which can meet the requirements of sample testing.