超高效液相色谱串联质谱法同时测定水中16种大环内酯和林可酰胺类抗生素  

Simultaneous determination of 16 macrolides and linconamides antibiotics in water by ultra performance liquid chromatography tandem mass spectrometry

作　　者：李敏[1] 黄梦凡 孙福红[2] 冯承莲[2] 常红 LI Min;HUANG Mengfan;SUN Fuhong;FENG Chenglian;CHANG Hong(College of Environmental Sciences&Engineering,Beijing Forestry University,Beijing,100083,China;State Key Laboratory of Environmental Criteria and Risk Assessment,Chinese Research Academy of Environmental Sciences,Beijing,100012,China)

机构地区：[1]北京林业大学环境科学与工程学院,北京100083 [2]中国环境科学研究院,环境基质与风险评估国家重点实验室,北京100012

出　　处：《环境化学》2024年第10期3297-3305,共9页Environmental Chemistry

基　　金：国家重点研发计划项目(2022YFC3201901);国家自然科学基金(42077306)资助.

摘　　要：据调查,大环内酯类抗生素(MAs)在我国所有抗生素中使用量居于首位、污染水平处于较高水平;林可霉素(林可酰胺类抗生素[LAs])是我国使用量最大的单个抗生素之一.鉴于两类抗生素抗菌作用类似,本研究建立了同时分析地表水中14种MAs以及2种LAs的超高效液相色谱串联质谱(UPLC-MS/MS)分析方法.水样萃取前添加0.5 g·L^(−1)Na2EDTA减少金属阳离子螯合影响,之后采用Oasis HLB固相萃取柱富集净化,最后以1%甲酸甲醇洗脱.UPLC-MS/MS测定采用甲醇和0.1%甲酸水作为流动相,根据质谱碎裂规律确定质谱定性定量离子对并采用多反应监测(MRM)模式进行分析.实际水样中目标抗生素的加标回收率为77%-114%,方法检出限绝大多数在0.004-0.06 ng·L^(−1)之间.方法应用于北京北运河和永定河的35个水样,检出8种MAs和2种LAs,浓度在0.01-71 ng·L^(−1)之间.总体来讲,北运河浓度高于永定河,北运河上游受纳污水处理厂出水可能是重要原因.两条河流检出物质浓度组成差异也较大,北运河主要是脱水红霉素A和罗红霉素,而永定河主要是脱水红霉素A.首次检出N-去甲基红霉素A,另外,螺旋霉素、麦迪霉素、林可霉素和氯林可霉素都普遍检出.Macrolide antibiotics(MAs)are the most commonly used antibiotics in China,with a relatively high level of pollution.Lincomycin,a kind of lincosamide antibiotics(LAs),is one of the most widely used individual antibiotics.In view of the similar antibacterial effects of the two types of antibiotics,an ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method was established for simultaneous analysis of 14 MAs and 2 LAs in surface water.0.5 g·L^(−1)of Na2EDTA was added to reduce the chelation effect of metal cations.Then antibiotics were extracted by Oasis HLB solid-phase extraction columns,eluted with 1%formic acid in methanol,and analyzed using UPLC-MS/MS under a multiple reaction monitoring(MRM)mode.Methanol and 0.1%formic acid in water were used as mobile phases.MS fragmentation patterns were studied to determine the qualitative and quantitative ion pairs.The results showed that the average recovery rates of target antibiotics in surface water ranged from 77%to 114%.The detection limit of the method was mostly in the range of 0.004-0.06 ng·L^(−1).This method was applied to 35 water samples from Beiyun River and Yongding River in Beijing,and 8 MAs and 2 LAs were detected with concentrations ranging from 0.01 ng·L−1 to 71 ng·L^(−1).Overall,the concentration level of antibiotics in the Beiyun River is higher than that of the Yongding River,and the effluent from the sewage treatment plant upstream of the Beiyun River may be an important source.The composition of antibiotics detected in the two rivers were also quite different,mainly dehydrated erythromycin A and roxithromycin in the Beiyun River,and dehydrated erythromycin A in the Yongding River.N-demethylerythromycin A was detected for the first time,and in addition,spiramycin,midecamycin,lincomycin,and chloramphenicol were generally detected.

关 键 词：新污染物 抗生素 大环内酯 林可酰胺 高效液相色谱质谱 地表水. 

分 类 号：X-1[环境科学与工程] O6[理学—化学]