水环境中磺胺类抗生素的超高效液相色谱-串联质谱法测定及其生态风险评估  

Determination and Ecological Risk Assessment of Sulfonamides in Environment Water by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：吴雯艳 胡红美[1] 何鹏飞 方益[1] 李铁军[1] 郭远明[1] WU Wen-Yan;HU Hong-Mei;HE Peng-Fei;FANG Yi;LI Tie-Jun;GUO Yuan-Ming(Key Laboratory of Mariculture and Enhancement of Zhejiang Province,Marine Fishery Institute of Zhejiang Province,Zhoushan 316021,China;School of Environmental Science and Engineering,Shanghai Jiao Tong University,Shanghai 200240,China)

机构地区：[1]浙江省海洋水产研究所,浙江省海洋渔业资源可持续利用技术研究重点实验室,舟山316021 [2]上海交通大学环境科学与工程学院,上海200240

出　　处：《分析化学》2024年第8期1182-1191,共10页Chinese Journal of Analytical Chemistry

基　　金：浙江省基础公益研究计划项目(No.LTGC24B050013);舟山市级基础研究项目(No.2024C31044)资助。

摘　　要：滥用和不合理使用抗生素已严重危及生态环境和人类健康。本研究建立了一种水环境中17种磺胺类抗生素(SAs)的全自动固相膜萃取-稳定同位素稀释-超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法,并将其用于自来水、河水和海水实际样品的检测,同时探讨了残留特征,评估了生态风险。取1 L含0.5 g/L Na2EDTA的水样(pH=3),采用3M SDB-XC膜片进行全自动固相膜萃取,洗脱液为10 mL甲醇-丙酮(1∶1,V/V)混合溶液,每6个样品前处理仅需60 min。本方法的线性检测范围为0.05~100μg/L,相关系数(R^(2))>0.999,检出限低至0.012~0.052 ng/L(S/N=3),回收率为76%~110%,相对标准偏差为0.5%~9.6%(n=5)。利用本方法检测实际样品中的SAs,在自来水中均未检出SAs,浙江舟山河水以及温州海域海水中分别检出3种和9种SAs,检出总浓度分别为0.875~21.826 ng/L和1.024~20.768 ng/L,均以磺胺甲恶唑(SMX)为主,分别占SAs总浓度的81%和74%。生态风险评估结果表明,在区域河水和海水中检出的SAs对3种营养级生物(藻类、大水蚤和鱼类)的风险商值(RQs)均小于0.01,生态风险较低。The abuse and irrational use of antibiotics in human veterinary medicine has seriously endangered the ecological environment and human health.In this study,a fully automatic solid-phase disk extraction-stable isotope dilution-ultra-high performance liquid chromatography-mass spectrometry method for determination of 17 kinds of sulfonamidesantibiotics(SAs)in water wasestablished,which was then applied to determination ofSAs in real samples including tap water,river water and seawater,respectively.Meanwhile,the residual characteristics were discussed and the ecological risks were assessed.With this method,1.0 L water sample with 0.5 g/L Na2EDTA(pH=3)was extracted and enriched by 3M SDB-XC disk,and eluted by 10 mL of mixture of methanol and acetone(1:1,V/V),and the pretreatment time of the sample was about 60 min per six samples.Under the optimized conditions,the linearity of the method for detection of 17 kinds of SAs ranged from 0.05 to 100μg/L,with correlation coefficients(R^(2))>0.999.In addition,the detection limits(S/N=3)were as lowas 0.012−0.052 ng/L,and the recoveries were in the range of 76%−110%,with relative standard deviations of 0.5%−9.6%(n=5).The results showed that no SAs was detected in tap water,while 3 and 9 kinds of SAs were detected in river water of Zhoushan,and seawater of Wenzhou Sea area in Zhejiang province,respectively.The total concentrations of the detected SAs were 0.875−21.826 ng/L and 1.024−20.768 ng/L in river water and seawater,respectively,and among which,sulfamethoxazole(SMX)was the predominant compound in river water and seawater,accounting for 81%and 74%of the total SAs,respectively.The ecological risk assessment showed that the risk quotients of the detected SAs in the river water and seawater in the study area for the three kinds of trophic organisms(algae,Daphnia and fish)were far less than 0.01,meaning that the ecological risk was low.

关 键 词：磺胺类抗生素 全自动固相膜萃取 超高效液相色谱-串联质谱法 水环境 生态风险 

分 类 号：O657.63[理学—分析化学] X832[理学—化学] X820.4[环境科学与工程—环境工程]