超高效液相色谱串联质谱测定中水中喹诺酮类抗生素  

Determination of Quinolones Antibiotics in Reclaimed Water by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometer

作　　者：王建凤[1,2] 王嘉琦[2] 刘喆[2] 王颖[2] 冯月超[2] 杜振霞[1] 贾丽[2] 范筱京[2] 

机构地区：[1]北京化工大学分析测试中心,北京100029 [2]北京市理化分析测试中心北京市食品安全分析测试工程技术研究中心,北京100089

出　　处：《中国给水排水》2018年第6期116-119,共4页China Water & Wastewater

基　　金：北京市科学技术研究院青年骨干人才计划(201615)

摘　　要：建立了检测中水中14种喹诺酮类抗生素残留的超高效液相色谱串联质谱(UPLCMS/MS)方法。水样通过HLB固相萃取小柱富集后,经C18色谱柱分离,运用乙腈-0.2%甲酸的10 mmol/L甲酸铵溶液进行梯度洗脱,质谱仪检测。采用电喷雾正模式电离(ESI+),多反应监测(MRM)模式进行检测,外标法定量。在1~100 ng/m L的线性范围内,各物质的线性关系良好,线性相关系数均≥0.991,方法的检出限为0.2~1.0 ng/L,定量限为0.5~2.0 ng/L,回收率稳定,RSD≤16%。该方法方便、准确,适用于中水中抗生素的痕量分析。A method for the determination of 14 quinolones antibiotics residues in reclaimed water by ultra performance liquid chromatography （UPLC-MS/MS） was developed. Water samples are firstly enriched by HLB solid phase extraction, then separated by C18 column and eluted with acetonitrile and 10 mmol/L ammonium formate solution with O. 2% formic acid included, the mass spectrometer is used for finally detection. The samples were ionized by positive electrospray ionization mode （ESI ＋ ）, detected by multiple reaction mode （ MRM）, and quantified by external standard method. In the range of 1 - 100 ng/mL, the regression equation of the antibiotics showed good liner relationship, and the linear correlation coefficients were no less than 0.991. The limits of detection and quantification were 0.2 - 1.0 ng/L and 0.5 - 2.0 ng/L respectively. As a result, the recoveries were stable, and the RSDs were less than 16%. The method is convenient and accurate, and could be applied to the trace analysis of antibiotics in reclaimed water.

关 键 词：中水 喹诺酮类 UPLC—MS/MS 

分 类 号：X832[环境科学与工程—环境工程]