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建立了膜透析/高效液相色谱-串联质谱法(MD/HPLC-MS/MS)检测畜产品中克伦特罗、莱克多巴胺、沙丁胺醇等9种β-受体激动剂的新方法。样品经乙酸铵缓冲液提取和β-葡萄糖苷醛甙酶/芳基硫酸酯酶酶解,采用标准再生纤维素膜(RC,截留分子量MWCO:1000D)透析净化,β-受体激动剂通过膜渗入透析液中,透析液用环已烷-乙酸乙酯(4:1)萃取,经Waters Xbridge C18色谱柱进行分离,以0.1%甲酸水和乙腈作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式进行检测,外标法定量。结果表明,9种β-受体激动剂在0.5~10μg/kg浓度范围内线性关系良好。方法的定量限为0.5μg/kg,在0.5、1.0、2.5μg/kg 3个添加水平的回收率为72.5%~92.6%,相对标准偏差(n=6)在4.1%~12.7%之间。该方法采用膜透析技术进行净化,无需使用昂贵的固相萃取柱,适用于畜产品中9种β-受体激动剂的经济、高灵敏度的分析检测。
A new method for the determination of 9 β-agonists such as clenbuterol, ractopamine and salbutamol in animal products by membrane chromatography / high performance liquid chromatography-tandem mass spectrometry (MD / HPLC-MS / MS) was established. Samples were extracted with ammonium acetate buffer and enzymatically digested with β-glucosidase / aryl sulfatase, dialyzed against standard regenerated cellulose membranes (RC, MWCO: 1000D), and β-receptor agonists were passed through membranes The dialysate was extracted with cyclohexane-ethyl acetate (4: 1), separated on a Waters Xbridge C18 column and eluted with 0.1% formic acid in water and acetonitrile as the mobile phase. The electrospray positive ion (ESI +) mode ionization, multiple reaction monitoring (MRM) mode for detection, external standard quantitative. The results showed that 9 kinds of β-agonists had good linearity in the range of 0.5 ~ 10μg / kg. The method has a limit of quantification of 0.5μg / kg. The recoveries at the three levels of 0.5,1.0,2.5μg / kg were 72.5% -92.6%. The relative standard deviations (n = 6) ranged from 4.1% to 12.7%. This method uses membrane dialysis for purification without the need for expensive solid-phase extraction columns and is suitable for the economical and sensitive analysis of nine beta-agonists in livestock products.