摘要
建立了同时检测11种β2-受体激动剂物质(包括沙丁胺醇、特布它林、塞曼特罗、塞布特罗、莱克多巴胺、克仑特罗、溴布特罗、苯氧丙酚胺、马布特罗、马贲特罗、溴代克仑特罗)在猪肉及猪肝脏中残留量的液相色谱-串联质谱(HPLC/MS-MS)方法。将样品粉碎后,用pH5.2的乙酸钠缓冲液提取,经β-盐酸葡萄糖醛苷酶-芳基硫酸酯酶水解,以高氯酸调节pH值,离心沉淀蛋白,分离得上清液用V(异丙醇):V(乙酸乙酯)=6;4的溶液萃取,再过阳离子交换柱净化,吹干后用高效液相色谱-串联质谱法测定,同时使用同位素内标(clenbuterol-D9、salbutamol-D3)进行定量分析。目标化合物的回收率在89.4%~110.5%,RSD为1.1%~2.8%,方法的最低检出限为0.25μg·kg^-1,能满足食品安全法规的需要。
The method for determination of β2-agonists (salbutamol, terbutaline, cimaterol, cimbuterol, ractompamine, clenbuterol, bromobuterol, isoxsuprine, mabuterol, mapenterol, bromclenbuterol) residues in liver and meat of pig was developed by HPLC/MS-MS. The sample was extracted in acetate buffer (pH 5.2), hydrolyzed by β-glucuronidase-aryl sulfatase. The protein was precipitated with perchloric acid. The extraction passed through a cation exchange column (MCX 3 mL, 60 mg), Clenbuterol-D9 & Salbutamol-D3 were used as an internal standard, then eleven β2-agonists can be determined at one time by HPLC/MS-MS. The experimental results from spiked liver sample indicate that the recoveries range from 89. 4%-110. 5% and the RSD is 1. 1%-2. 8%. The limits of detection (LODs) is 0.25μg· kg^-1. The method is suitable for food safety.
出处
《质谱学报》
EI
CAS
CSCD
2007年第4期193-201,共9页
Journal of Chinese Mass Spectrometry Society