固相萃取-超高效液相色谱-三重四极杆质谱法测定海水中14种喹诺酮类抗生素  

Determination of 14 quinolones in seawater using solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：宋晓娟 李婷婷 赵颖 杨维英 SONG Xiaojuan;LI Tingting;ZHAO Ying;YANG Weiying(Lianyungang Environmental Monitoring Center of Jiangsu Province,Lianyungang 222001,Jiangsu,China)

机构地区：[1]江苏省连云港环境监测中心,江苏连云港222001

出　　处：《化学研究》2023年第4期319-327,332,共10页Chemical Research

基　　金：江苏省2021年环境监测科研基金项目计划(2120)。

摘　　要：本研究采用固相萃取-超高效液相色谱-三重四极杆质谱联用技术,建立了海水中14种喹诺酮类抗生素的分析方法。将海水样品调至pH=2.0,加入0.5 g/L Na_2EDTA,经HLB固相萃取柱富集后,用甲醇洗脱,采用多反应监测模式进行检测。结果表明,14种喹诺酮类抗生素标准溶液线性关系良好,相关系数在0.9987~0.9999之间,以清洁海水为基质进行高、低浓度加标实验,回收率在74.9%~109.7%之间,精密度在4.7%~13.6%之间,符合质控要求。该方法检出限在0.015~0.561 ng/L之间,能够满足痕量分析要求。实样分析表明,该方法能够成功应用于海水中痕量喹诺酮类抗生素的分析,方法稳定可靠。A method for the determination of 14 quinolones in seawater was developed by using solid phase extraction(SPE)and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Various parameters were optimized by comparing the sample recoveries under different conditions.Samples were efficiently extracted at pH 2.0 after adding 0.5 g/L Na 2 EDTA.All the 14 quinolones were enriched by HLB cartridges,eluted with methanol,and then detected by multiple reaction monitoring(MRM)modes.The results show that the linear relationships of the 14 quinolones are good with the correlation coefficients range from 0.9987 to 0.9999.The average recoveries of the target compounds in clean seawater spiked at high and low concentrations range from 74.9%to 109.7%,and the relative standard deviations ranged from 4.7%to 13.6%.The limits of detections for the target analytes are in the range of 0.015-0.561 ng/L.It proves that,the developed method is suitable for the detection of trace quinolones in seawater samples.The method is reliable and acceptable.

关 键 词：喹诺酮类抗生素 固相萃取 超高效液相色谱-串联质谱 海水 

分 类 号：O657[理学—分析化学]