SPE-RRLC-MS/MS测定河水和沉积物中14种典型抗生素  

Determination of 14 antibiotics in water and sediment by SPE-RRLC-MS/MS

作　　者：吕凯 刘晓薇[1,2] 邓呈逊[3] 郑坤[3] 李兰兰[1,2] 史江红 郭伟 LYU Kai;LIU Xiaowei;DENG Chengxun;ZHENG Kun;LI Lanlan;SHI Jianghong;GUO Wei(School of Resources and Environmental Engineering,Hefei University of Technology,Hefei,230009,China;Key Laboratory of Nanominerals and Pollution Control of Anhui Higher Education Institutes,Hefei University of Technology,Hefei,230009,China;China Department of Biological and Environmental Engineering,Hefei University,Hefei,230022,China;Guangdong Provincial Key Laboratory of Soil and Groundwater Pollution Control,School of Environmental Science and Engineering,Southern University of Science and Technology,Shenzhen,518055,China)

机构地区：[1]合肥工业大学资源与环境工程学院,合肥230009 [2]合肥工业大学纳米矿物与污染控制安徽普通高校重点实验室,合肥230009 [3]合肥学院生物与环境工程系,合肥230022 [4]南方科技大学环境科学与工程学院广东省土壤与地下水防控及修复重点实验室,深圳518055

出　　处：《环境化学》2019年第11期2415-2424,共10页Environmental Chemistry

基　　金：国家自然科学基金(51609058);中国博士后基金(2016M602009);合肥学院科研发展基金(18ZR03ZDA);国家重点研发计划(2018YFC1801603);深圳市科技创新委员会(CYJ20160301114534506)~~

摘　　要：针对磺胺类、喹诺酮类、四环素类、大环内酯类共14种典型抗生素,建立了水和沉积物中固相萃取-高分离快速液相色谱-串联质谱(SPE-RRLC-MS/MS)前处理方法和仪器检测方法.14种抗生素在5-100μg·L^-1范围内线性良好,相关系数r≥0.990.优化后的前处理方法采用乙腈/0.1 mol·L^-1 EDTA-Mcllvaine(1∶1,V/V)作为沉积物样品中目标抗生素的提取剂,甲醇/丙酮(85∶15,V/V)作为固相萃取柱的洗脱液.表层水中14种抗生素的加标回收率为56%-117%,相对标准偏差(n=3)为0.10%-12%;沉积物中14种抗生素的加标回收率为57%-127%,相对标准偏差(n=3)为0.10%-25%.表层水和沉积物中抗生素的方法检出限分别为0.18-5.88 ng·L^-1和0.25-2.94 ng·g^-1.该方法用于检测合肥市南淝河表层水和沉积物中的抗生素,5种抗生素被检出,浓度范围分别为32-308 ng·L^-1和2.70-329 ng·g^-1.A solid phase extraction-high separation rapid liquid chromatography-tandem mass spectrometry(SPE-RRLC-MS/MS) method was developed to simultaneously determinate 14 typical antibiotics including sulfonamides, quinolones, tetracycline and macrolides in water and sediments. The pretreatment process was improved to obtain high recoveries. The mixture of acetonitrile/0.1 mol·L^-1 EDTA-Mcllvaine(1∶1, V/V) was selected as the extraction solvent of antibiotics in the sediment samples. The mixture of methanol/acetone(85∶15, V/V) was used to elute these target antibiotics. The results showed that the linear range of the 14 antibiotics was between 5-100 μg·L^-1(r ≥ 0.990). The recovery and relative standard deviation(RSD, n=3) of 14 antibiotics in surface water were 56%-117% and 0.10%-12%, respectively. The recovery and RSD(n=3) of 14 antibiotics in sediments were 57%-127% and 0.10%-25%, respectively. The detection limit of these antibiotics in surface water and sediments ranged from 0.18 ng·L^-1 to 5.88 ng·L^-1 and from 0.25 ng·g^-1 to 2.94 ng·g^-1, respectively. The method was applied to detect antibiotics in the Nanfei River, Hefei City. Five antibiotics were detected in surface water and sediments in the ranges of 32-308 ng·L^-1 and 2.70-329 ng·g^-1, respectively.

关 键 词：抗生素 固相萃取 高分离快速液相色谱-串联质谱 河水 沉积物 南淝河 

分 类 号：O65[理学—分析化学]