猪肉中特布他林等4种瘦肉精残留量的固相萃取-气相色谱质谱联用测定法

Determination of four clenbuterol residues in pork by solid phase extraction and gas chromatography-mass spectrometry

目的建立气相色谱质谱联用固相萃取法测定猪肉中特布他林等4种瘦肉精残留量的检测方法。方法将猪肉去筋切碎后,称取一定量的试样,经过提取、固相萃取、衍生、溶解后,于气相色谱-质谱联用仪中进样测定。结果 HP-5MS毛细管柱对4种瘦肉精残留量能达到很好的分离效果,方法检出限为0.4-0.7μg/kg,定量限为1.3-2.3μg/kg（取样量为5.0 g计算）,回收率为75.5%-89.6%,精密度范围为2.5%-4.2%,相关系数〉0.999 0。结论该方法能获得满意的分离效果,并具有较高的灵敏度和精密度,回收率也满足方法学要求,完全适合于猪肉中特布他林、克伦特罗、沙丁胺醇、莱克多巴胺等4种瘦肉精残留的检测。

[Objective]To establish a method for the determination of four clenbuterol residues,such as terbutaline,in pork by solid phase extraction and gas chromatography-mass spectrometry（GC-MS）.[Methods]The pork was treated by removing the ribs and chopping, to weighing a sample. After solid phase extraction, derivatization and dissolution, the sample was determined by GC-MS.[Results]Four clenbuterol residues were satisfactorily separated by using HP-5MS capillary column. The limit of detection（LOD）of this method was 0.4-0.7 μg/kg,and the limit of quantification（LOQ）was 1.3-2.3 μg/kg（sampling amount of 5.0 g）.The recoveries were 75.5%-89.6%. The precision was between 2.5% and 4.2%,while the correlation coefficient was greater than0.999 0. [Conclusion]This method has satisfactory separation with high sensitivity and precision,and the recovery meets the methodological requirements. Above all,this method is entirely suitable for the simultaneous determination of four clenbuterol residues,including terbutaline,clenbuterol,salbutamol and lake dopamine.