高效液相色谱-串联质谱法测定猪肉中9种β_2-受体激动剂残留量  

Determination of 9 β_2-Agonists Residuals in Pork by HPLC-MS/MS

作　　者：潘艳坤[1] 张兰[1] 杨益林[1] 叶开富[1] 张思敏[1] 韦英亮[1] 

机构地区：[1]广西分析测试研究中心,南宁530022

出　　处：《理化检验（化学分册）》2015年第3期360-364,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：广西科学研究与技术开发计划项目(桂科重122203-2-2)

摘　　要：采用高效液相色谱-串联质谱法测定了猪肉中9种β-受体激动剂的残留量。样品经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解后加入高氯酸沉淀蛋白并离心,取上清液过PCX阳离子固相萃取小柱净化,用氨水-甲醇(5+95)混合液洗脱,氮气吹干后用乙腈定容至1 mL。以CAPCELL PAK CR色谱柱为分离柱,以10mmol·L-1乙酸铵溶液-乙腈(55+45)混合溶液(含体积分数为0.1%的甲酸)为流动相进行洗脱,采用电喷雾正离子源及选择反应监测模式进行测定,内标法进行定量。9种β-受体激动剂的质量浓度在4.00~100μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.09~0.50μg·L-1之间。对空白样品进行加标回收试验,回收率在83.2%~102%之间,测定值的相对标准偏差(n=6)在5.0%~12%之间。The HPLC-MS/MS was used to determine 9β2-agonists residuals in pork.The sample was hydrolyzed byβ-glucuronidase/aryl sulfatase.The protein was precipitated with perchloric acid and removed by centrifugation.The supernatant was purified by PCX solid phase extraction column with a mixture of ammonia and methanol(5+95)as eluent.The eluate was dried under N2 stream,then the residue was dissolved with 1 mL acetonitrile.The CAPCELL PAK CR column was used as stationary phase and the mixture(contain 0.1%φ)of10mmol·L-1 ammonium acetate and acetonitrile(55+45)was used as mobile phase for elution.ESI+and SRM were adopted in MS/MS.The linear relationship between the peak area and the mass concentration of the 9β2-agonists was in the range of 4.00-100μg·L-1,with detection limits(3S/N)in the range of 0.09-0.50μg·L-1.Recovery rates measured by standard addition method were in the range of 83.2%-102% with RSD′s(n=6)in the range of 5.0%-12%.

关 键 词：高效液相色谱-串联质谱法 Β2-受体激动剂 猪肉 

分 类 号：O657.63[理学—分析化学] TS251.51[理学—化学]