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低延迟体积模式液相色谱-串联质谱法检测猪肉中盐酸克伦特罗残留量

Determination of Clenbuterol Residues in Pork by Liquid Chromatography-Tandem Mass Spectrometry with Low Delay Volume Mode

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【作者】 张厚森杨凤岩周存山朱成晶贾涛李新丽赵厚民

【Author】 ZHANG Hou-sen1,YANG Feng-yan1,ZHOU Cun-shan*2,ZHU Cheng-jing1 JIA Tao1,LI Xin-li1,ZAHO Hou-min1(1.Nutrients and Toxic Testing Center of Jiangsu Province,Physics and Chemistry Testing Center of Jiangsu Province,Nanjing 210042; 2.College of Food and Biological Engineering,Jiangsu University,Zhenjiang 212013)

【机构】 江苏省理化测试中心江苏省营养成分与有毒有害物质检测中心江苏大学食品与生物工程学院

【摘要】 应用高效液相色谱-串联质谱法(HPLC-MS/MS),在液相部分采用低延迟体积模式,以盐酸克伦特罗-D9为内标,建立了快速测定猪肉中盐酸克伦特罗残留的检测方法。样品经过提取纯化后,采用C18色谱小柱进行梯度洗脱分离,电喷雾正离子MRM质谱检测。低延迟体积模式可实现洗脱液的快速梯度变换,仪器检测时间为2.0min;盐酸克伦特罗的保留时间为0.82min,其保留时间重现性好,所建立的标准曲线线性较好(R2=0.9993)。该方法的定量限(LOQ)为0.5μg/kg;当加标量为0.5、5、10μg/kg时,其回收率为81.2%~114.2%,相对标准偏差为6.4%~11.1%(n=6)。该方法检测速度快、灵敏度高、结果准确,可以满足实验室对猪肉中盐酸克伦特罗残留的高通量测试。

【Abstract】 A liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for rapid determination of clenbuterol residues in pork by using clenbuterol-D9 as the internal standard was established.The pretreated samples were separated on a C18 column(50×2.1 mm,1.8 μm) and finally detected by positive electrospray ionization spectrometry(ESI+) with MRM mode.The detection time was 2.0 min and the retention time of clenbuterol was only 0.82 min.The limit of quantification of the method was 0.5 μg/kg.When spiked at 0.5 μg/kg,5 μg/kg and 10 μg/kg,the recoveries of clenbuterol ranged from 81.2% to 114.2%,with the relative standard deviations of 6.4%-11.1%(n=6).This method is characteristic of rapidity,high sensitivity and precision and can used for pork clenbuterol residues determination in high-throughput testing.

【基金】 高级人才启动项目(12JDG074);青年骨干培养工程
  • 【文献出处】 分析科学学报 ,Journal of Analytical Science , 编辑部邮箱 ,2013年02期
  • 【分类号】S859.84
  • 【被引频次】1
  • 【下载频次】109
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