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超高效液相色谱-串联四极杆质谱法测定麻辣烫中喹诺酮类药物残留
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作者单位
赵飞,高广慧,贾宏新 辽宁省食品检验检测院 
基金项目:国家质检总局科研计划项目(2016IK169)
中文摘要:建立了麻辣烫中14种喹诺酮类药物残留的超高效液相色谱-串联四极杆质谱(UPLC-MS/MS)检测方法。采用酸化乙腈提取麻辣烫中的喹诺酮类药物残留,提取溶液经盐析和C18固相萃取柱净化后,在电喷雾离子源中正离子模式下,采用多反应监测(MRM)方式进行测定,内标法定量。结果显示,14种喹诺酮类药物在7.5~100 μg/L范围内线性关系良好,相关系数均大于0.990。在3个不同加标水平下的平均回收率为75.4%~110.0%,相对标准偏差(n=6)为1.3%~10.1%,14种化合物的检出限和定量下限分别为0.5,1.5 μg/kg。该方法操作简单、快速,净化效果好,灵敏度高,适用于麻辣烫中多种喹诺酮类药物残留的同时定性和定量检测。
中文关键词:固相萃取  超高效液相色谱-串联四极杆质谱法  喹诺酮类药物  麻辣烫
 
Determination of Quinolones in Hotpot Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of 14 quinolones in hotpot.Samples were extracted with acidified acetonitrile,defated with n hexane,separated on a C18 solid phase extraction(SPE) column,and analyzed by LC-ESI-MS/MS under the positive mode with multiple reaction monitoring(MRM).The method showed good linearities for 14 quinolones over the range of 7.5-100 μg/L with correlation coefficients(r) more than 0.990.The detection limits of 14 quinolones were 0.5 μg/kg,and the quantitation limits were 1.5 μg/kg.The recoveries of all analytes in hotpot ranged from 75.4% to 110.0%with relative standard deviations(RSD,n=6)of 1.3%-10.1%.The method has the advantages of simplicity,rapidness,good purifying effect and sensitivity,and is suitable for the simultaneous determination of quinolones in hotpot.
Key Words:SPE  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  quinolones  hotpot
引用本文:赵飞,高广慧,贾宏新.超高效液相色谱-串联四极杆质谱法测定麻辣烫中喹诺酮类药物残留[J].分析测试学报,2017,36(6):768-772.
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