液相色谱质谱法测定地表水中3种广谱抗菌剂  

Determination of Three Wide-spectrum Antibiotic in Surface Water by Liquid Chromatography Mass Spectrometry

作　　者：陈峰[1] 郭佳惠 张宝锋 何平[1] 王奕奕[1] 周姗[1] 沈建东[1] CHEN Feng;GUO Jiahui;ZHANG Baofeng;HE Ping;WANG Yiyi;ZHOU Shan;SHEN Jiandong(Hangzhou Environmental Monitoring Center Station,Hangzhou 310007,China)

机构地区：[1]杭州市环境监测中心站,浙江杭州310007

出　　处：《环境科学与技术》2021年第1期224-227,共4页Environmental Science & Technology

基　　金：杭州市农业和社会发展科研项目(20191203B66);杭州市农业和社会发展科研项目(20191203B65);杭州市“131”中青年人才培养计划(2016-2020年)。

摘　　要：该文探讨了固相萃取/液相色谱-电喷雾串联质谱联用技术(SPE/LC-ESI-MS/MS)分析水中氟康唑、甘宝素和卡巴氧等3种广谱抗菌剂的方法,样品通过SPE提取,采用Agilent ZORBAX SB-C_(18)色谱柱,流动相采用0.1%甲酸乙腈和0.1%甲酸水,梯度洗脱,正离子多反应监测模式下电喷雾离子源电离后进行定性和定量分析。3种化合物在0~100μg/L浓度范围内线性良好,相关系数0.999 6~0.999 9,方法检出限为0.13~0.49 ng/L;低、中、高3个添加水平下实际样品加标回收率范围为75.7%~93.8%,相对标准偏差为5.8%~14.5%。用该方法检测杭州市68个地表水样品中的目标物浓度,多数可检出。A method has been researched for the determination of three wide-spectrum antibiotic in surface water by solid phase extraction-liquid chromatography-electrospray ionization tandem mass spectrometry(SPE/LC-ESI-MS/MS). The samples were extracted by solid phase extraction. Liquid chromatography separation was performed by an Agilent ZORBAX SB-C_(18) column utilizing a gradient elution program of acidified water(containing 0.1% formic acid) and acidified acetonitrile(containing 0.1% formic acid) as the mobile phase. Qualitative and quantitative analysis was achieved by LC-ESIMS/MS in multiple reactions monitoring and positive mode. Good linearity was performed in the range of 0~100μg/L with correlation coefficients from 0.999 6 to 0.999 9,limit of detection(LOD) for the three wide-spectrum antibiotic was in the ranges of 0.13~0.49 ng/L. At three different concentration levels, the average recoveries of 3 target compounds in spiked practical samples ranged from 75.7% to 93.8% with the relative standard deviations between 5.8% and 14.5%. The method was applied to detect the concentration of compounds in 68 samples of surface water in Hangzhou, most of which were detected.

关 键 词：广谱抗菌剂 固相萃取 地表水 液相色谱-电喷雾串联质谱 

分 类 号：X832[环境科学与工程—环境工程]