液质联用仪测定动物源性食品中11种β_2-受体激动剂的研究

Determination of 11 β_2-agonists in Foodstuff of Animal Origin by Liquid Chromatograph with Tandem Mass Spectrometric Detection

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.