气相色谱-质谱法同时测定动物性食品中8种β-兴奋剂的残留量

Simultaneous determination of 8 β-agonists in animal food by GC/MS

目的:应用OasisMCX固相萃取净化、气相色谱-质谱同时测定动物组织样品中8种β-兴奋剂(克伦特罗、沙丁胺醇、妥布特罗、特布它林、喷布特罗、心得安、倍他索洛尔、非诺特罗)的残留量。方法:样品粉碎后经β-葡萄糖醛苷酶水解用乙酸钠缓冲溶液提取,MCX固相萃取柱进一步净化,再用N,O双(三甲基硅基)三氟乙酰胺-三甲基氯硅烷(BSTFA+TMCS,99+1)衍生化,用美托洛尔(metoprolol)为内标。采用选择离子监控模式(SIM)检测,GC/MS测定分析。结果:8种β-兴奋剂不同水平的加标回收率范围为51.9%～101.7%(n=6),相对标准偏差为2.7%～16.0%(n=6)。结论:本方法操作简单,灵敏度高,选择性和重复性好。

Objective:To develop a method for the simultaneous determination of clenbuterol, salbutamol, tulobuterol, terbutalin, penbutolol, propranolol, betaxolol, fenoterol residues in animal tissue using gas chromatography/mass spectrometry(GC/MS) .Methods:The homogenized samples were digested by β-glucuronidase enzyme, and extracted with sodium acetate.Further cleanup was performed on a MCX cartridge and the purified drugs were derivatized with \[N,O-bis (trimethylsilyl) trifluoroacetamide (BSTFA)-trimethylchlorosilane (TMCS),99+1\], metoprolol was used as internal standard.Selected ion monitoring (SIM) method was applied for detection.Results:The rates of recovery were 51.9%~101.7%(n=6),and the relative standard deviations were 2.7%~16.0%(n=6).Conclusion:The method is simple,sensitive,selective and reproducible.