反相液相色谱-串联质谱法检测猪肝中26种β_2-受体激动剂类药物残留  

Determination of Residues of 26 β_2-Agonists in Pork Liver by Reversed Phase High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘佳 谢云峰 任丹丹 崔兴品 梁桂荣 杨永坛 

机构地区：[1]中粮营养健康研究院,北京市营养健康与食品安全重点实验室,北京102209

出　　处：《分析化学》2014年第10期1486-1492,共7页Chinese Journal of Analytical Chemistry

基　　金：中粮集团有限公司年度科技计划项目(No.2012-C2-F012)资助

摘　　要：建立了一种猪肝中26种β2-受体激动剂药物残留的反相液相色谱-串联质谱（ HPLC-MS/MS）检测方法。样品经β-葡萄糖苷酸酶/芳基硫酸酯酶酶解12 h 后,加入 HClO4调至 pH 1,去除蛋白,残渣经过0.1 mol/L HClO4再次提取后,合并提取液,调节混合提取液至pH 4,过混合阳离子（ MCX）固相萃取柱净化。采用0.1%甲酸（A）和0.1%甲酸-乙腈（B）作为流动相进行梯度洗脱,质谱（ESI＋）采用多离子检测模式（ MRM）对β2-受体激动剂的定量离子和定性离子进行监测,本方法在15 min内完成26种目标化合物的分离分析。26种β2-受体激动剂在5、10和20μg/L添加水平的回收率为64.0%～112.7%,相对标准偏差小于15.2%,方法检出限为0.15～1.35μg/kg。A method for determination of residues of 26 β2-agonists in pork liver was developed using high performance liquid chromatography with tandem mass spectrometric （ HPLC-MS/MS ） . After enzymatic hydrolysis with β-Glucuronidase/Arylsulfatase for 12 hours, the pH of sample solution was adjusted to 1 using＆amp;nbsp;perchloric acid for protein precipitation. The precipitate was extracted with 0. 1mol/L perchloric acid aqueous. The extracts in the above two steps were combined and adjusted to pH 4 for the solid phase extraction （ MCX） . And then the 26 β2-agonists residues in the extracts were separated on a reversed phase HPLC column using a gradient elution program of 0. 1% formic acid aqueous solution （A） and 0. 1% formic acid in acetonitrile solution （ B） . Multiple reaction monitoring （ MRM） with positive polarity was selected to monitor qualitative and quantitative ion. Based on the optimized method, 26 β2-agonists could be analyzed in 15 min. The recoveries ranged from 64 . 0% to 112 . 7% for the 26 kinds ofβ2-agonists residues with three spiked levels of 5, 10 and 20 μg/kg. The relative standard deviations （ RSDs） were less than 15. 2%. The limits of detection （LOD） for the 26 kinds of β2-agonists were 0. 15-1. 35 μg/kg.

关 键 词：Β2-受体激动剂 液相色谱-串联质谱仪 猪肝 残留 

分 类 号：O657.63[理学—分析化学]