通过型固相萃取-超高效液相色谱-串联质谱法检测火锅底料中的喹诺酮类药物

Detection of Quinolones in Hotpot Seasoning by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

[目的]建立通过型固相萃取-超高效液相色谱-串联质谱法测定火锅底料中11种喹诺酮类药物的分析方法。[方法]样品用酸化乙腈提取,经Oasis Prime HLB固相萃取柱净化,收集流出液,用超高效液相色谱-串联质谱仪多反应监测扫描模式检测和同位素内标定量。[结果]所有目标物在线性范围内线性良好,相关系数≥0.99,检出限为0.6~4.8μg/kg,定量限为2.0~13.2μg/kg,不同加标水平的平均回收率为78.5%~103.4%,相对标准偏差为2.8%~9.1%。[结论]该方法具有快速、准确、灵敏度高的特点,可用于火锅底料中11种喹诺酮类药物的测定。

[Objective]The research aimed to establish an analytical method for the determination of 11 quinolones in hotpot seasoning by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry.[Method]Samples were extracted with acidic acetonitrile,cleaned-up by solud-phase extraction using Oasus Prime HLB column.The analytes were detected in the multi-reaction monitoring(MRM)mode and quantified by the isotope internal standard method.[Result]The calibration curves were linear well in the corresponding concentration ranges,with correlation coefficient≥0.99.The limits of detection and quantification were 0.6-4.8μg/kg and 2.0-13.2μg/kg,respectively.The average recoveries at three spiked levels ranged from 78.5%to 103.4%with RSD of 2.8%-9.1%.[Conclusion]This method is rapid,accurate and sensitive.It can be used for the determination of 11 quinolones in hotpot seasoning.