地表水中的抗生素质谱指纹提取方法的研究  

Development of Mass Spectrum Fingerprint Extraction Technology for Antibiotics in Surface Water

作　　者：陈思祎 郭欣妍[2] 朱伟[2] 王娜[2] 王瑛[1] 孔德洋[2] 

机构地区：[1]南京理工大学化工学院,南京210094 [2]环境保护部南京环境科学研究所,南京210042

出　　处：《分析化学》2018年第2期178-187,共10页Chinese Journal of Analytical Chemistry

基　　金：本文系2016环保公益性行业科研专项《典型饮用水源地抗生素污染源解析技术研究》、国家自然科学基金项目(No.21507037)和环保公益性行业科研专项(No.201309031)资助

摘　　要：从固相萃取柱、上样样品p H值、洗脱液、定容液四方面优化前处理流程,建立了地表水中喹诺酮类、磺胺类、四环素类、大环内酯类、青霉素类、头孢菌素类以及氨基糖苷类7类共49种抗生素的质谱指纹的提取方法。水样采用MAX-HLB串联柱富集净化,在超高效液相色谱-串联质谱(UPLC-MS/MS)的多反应监测(MRM)模式下进行定性及定量分析。结果表明,各抗生素在0.001~0.5μg/m L(链霉素为0.01~5μg/m L)浓度范围内线性关系良好,各目标抗生素的加标回收率为51.7%~94.8%,相对标准偏差为2.2%~9.7%。以3倍和10倍信噪比确定目标抗生素在两种定容液中的检出限以及定量限分别为0.01~3.23μg/L和0.05~3.43μg/L以及0.04~10.8μg/L和0.17~11.4μg/L。应用此方法对秦淮河和玄武湖的9个位点进行了抗生素污染筛查。An extract method for the fingerprint feature of 49 kinds of antibiotics belonging to multiple classes in surface water was developed. Water sample was purified and concentrated by tandem dual column( MAX and HLB),and qualitatively and quantitatively analyzed by ultra-high performance liquid chromatographytandem mass spectrometric( SPE-UPLC-MS/MS) under multiple reaction monitoring( MRM) mode. The pretreatment was optimized in types of SPE column,loading p H,eluent and redissolution for multiclass antibiotics. The results showed that the linearity of target antibiotics was good in the range of 0. 001-0.5 μg/m L( 0.01-5 μg/m L for streptomycin). The recoveries were from 51.7% to 94.8%,and the relative standard deviations( RSDs) ranged from 2. 19% to 9. 67%. The limits of detection( LOD,S/N = 3) were0.01-3.23 μg/L and 0. 05-3. 43 μg/L and the limits of quantification( LOQ,S/N = 10) were 0. 04-10.8 μg/L and 0.17-11.4 μg/L in different redissolve solutions. This method was applied to the determination of antibiotics in water samples from 9 sites of Qinhuai River and Xuanwu Lake.

关 键 词：固相萃取 超高效液相色谱-串联质谱 抗生素 地表水 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]