分子印迹固相萃取/超高效液相色谱-串联质谱法同时测定动物源性食品中11种β-受体阻断剂残留  

Determination of Eleven β-Blocker Residues in Animal Derived Foods by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry with Molecularly Imprinted Solid Phase Extraction

作　　者：郝杰 姜洁 邵瑞婷 丁学妍 史娜 路勇 

机构地区：[1]北京市食品安全监控和风险评估中心,北京100041

出　　处：《分析测试学报》2016年第10期1278-1282,共5页Journal of Instrumental Analysis

基　　金：北京市科技计划(Z161100000616007)

摘　　要：建立了一种分子印迹固相萃取/超高效液相色谱-串联四极杆质谱法同时测定动物源性食品中11种β-受体阻断剂残留量的方法。样品经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解后,上清液调节p H值,以异丙醇-乙酸乙酯(5∶5,体积比)萃取,有机相吹干后复溶过分子印迹固相萃取柱净化。样品经BEH C_(18)色谱柱分离,以甲醇-5 mmol/L乙酸铵水溶液(含0.1%甲酸)进行梯度洗脱,电喷雾电离正离子模式下采用多反应监测,基质加标曲线定量。11种β-受体阻断剂在0.05~10μg/kg范围内线性关系良好,相关系数均不小于0.991,方法检出限和定量下限分别为0.02~0.1μg/kg和0.05~0.25μg/kg。在猪肉、猪肝基质中3个添加水平下,平均回收率分别为73.2%~108.3%及70.2%~98.2%,相对标准偏差分别为1.3%~9.5%及3.7%~9.8%。该方法快速、灵敏、准确,适用于β-受体阻断剂多组分残留的测定。A molecularly imprinted solid phase extraction coupled with ultra high performance liquid chromatography- tandem mass spectrometric （UPLC -MS/MS） method was developed for the deter- mination of eleven beta blocker residues in animal derived foods. The sample was enzymed with ,β- glucuronidase/aryl sulfatase. The supernatant fraction was adjusted to the optimal pH value, and then extracted with isopropanol - ethyl acetate （5 ： 5, by volume）. The organic solvent was first e- vaporated to dryness, and then redissolved, finally purified by molecularly imprinted solid phase ex- traction. The analyte was separated with a BEH C18 column by gradient elution using methanol -5 mmol/L ammonium acetate （containing 0. 1% formic acid） as mobile phase, and detected by MS under ESI ＋ ionization and multiple reactions monitoring mode. The quantification of the analytes was performed by the matrix standard addition method. The limits of detection and limits of quantitation were in the ranges of 0.02 -0. 1 p^g/kg and 0.05 -0. 25 p^g/kg, respectively. The calibration curves of 11 ,β-blockers were linear in the range of 0.05 - 10 μg/kg, with correlation coefficients not less than 0. 991. Under three spiked levels, the average recoveries of the analytes in pork and liver were 73.2% - 108.3% and 70. 2% - 98.2% , respectively, with relative standard deviations of 1.3% -9.5% and 3.7% -9.8% , respectively. The method is rapid, sensitive and precise, and is suitable for the determination of,β-blocker multi residues in animal derived foods.

关 键 词：分子印迹固相萃取 液相色谱-串联质谱法 Β-受体阻断剂 残留检测 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]