在线固相萃取-同位素稀释/超高效液相色谱-串联质谱法测定蜂蜜中26种喹诺酮类化合物  

Simultaneous Determination of 26 Quinolones in Honey by UPLC-MS/MS with On-line Solid-phase Extraction and Isotope Dilution

作　　者：张居舟 李静 ZHANG Ju-zhou;LI Jing(Anhui Provincial Institute for Food and Drug Control,Hefei 230051,China;China National Center for Quality Supervision and Test of Agricultural-Avocation Processed Food,Hefei 230051,China)

机构地区：[1]安徽省食品药品检验研究院,安徽合肥230051 [2]国家农副加工食品质量检验检测中心,安徽合肥230051

出　　处：《分析测试学报》2021年第10期1417-1424,共8页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2017YFC1601705)。

摘　　要：建立了在线固相萃取/超高效液相色谱-串联质谱(SPE/UPLC-MS/MS)同时测定蜂蜜中26种喹诺酮类化合物的方法。样品用1%甲酸溶液-甲醇(10∶90)提取,经OasisPRiMEHLB固相萃取柱快速净化后,采用AgilentEclipsePlusRRHDC_(18)柱(2.1 mm×50 mm,1.8μm)分离,以0.1%甲酸溶液-乙腈为流动相梯度洗脱。在电喷雾离子源正离子模式下,采用动态多反应监测(dMRM)模式,内标法定量。结果表明,26种喹诺酮类化合物在各自的质量浓度范围内均呈良好线性关系,相关系数(r^(2))均大于0.997,定量下限(LOQ)为0.5~2.0μg/kg;在低、中、高3个加标水平下,平均回收率为79.5%~110%,相对标准偏差(RSD)为2.0%~12%。该方法简便、快捷、高效,适用于蜂蜜中喹诺酮类化合物的筛查及定量测定。An on-line solid-phase extraction/ultra performance liquid chromatography-tandem mass spectrometric(SPE/UPLC-MS/MS)method was developed for the determination of twenty-six quino⁃lone residues in honey.Firstly,the samples were extracted with 1%formic acid solution-methanol(10∶90),then rapidly purified by solid-phase extraction using an Oasis PRiME HLB cartridge.During the process,the key factors,such as the extraction solvent and purification method were opti⁃mized individually.The analytes were separated on an Agilent Eclipse Plus RRHD C_(18) column(2.1 mm×50 mm,1.8μm)by gradient elution,using water containing 0.1%formic acid and ace⁃tonitrile as the mobile phases.The target compounds were analyzed with electrospray ion source in positive ion mode under dynamic multi-reaction monitoring(dMRM)mode,and quantified by inter⁃nal standard method.Results showed that there were good linear relationships for 26 quinolones in their respective concentration ranges with correlation coefficients(r^(2))more than 0.997.The limits of quantitation(LOQ)were in the range of 0.5-2.0μg/kg.The average recoveries for 26 quinolones at low,medium and high spiked levels ranged from 79.5%to 110%,with relative standard devia⁃tions(RSD,n=6)of 2.0%-12%.The developed method was rapid and accurate,which was suit⁃able for the simultaneous screening and quantitative determination of 26 quinolones in honey.

关 键 词：在线固相萃取 超高效液相色谱-串联质谱法 喹诺酮类 蜂蜜 

分 类 号：O657.7[理学—分析化学] TS201.6[理学—化学]