三聚氰胺/邻苯二甲醛共价有机骨架材料结合固相萃取-液相色谱串联质谱检测环境水样中痕量磺胺类抗生素  

Melamine/o-Phthalaldehyde Covalent Organic Frameworks for Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry Analysis of Sulfonamide Antibiotics in Environmental Samples

作　　者：王欣梅[1,2] 徐桂菊 王晓利 王霞[2] 王明林[1] 赵汝松[2] 林金明[3] WANG Xin-Mei;XU Gui-Ju;WANG Xiao-Li;WANG Xia;WANG Ming-Lin;ZHAO Ru-Song;LIN Jin-Ming(College of Food Science and Engineering,Shandong Agricultural University,Taian 271018,China;Analysis and Test Center,Shandong Academy of Sciences,Jinan 250014,China;Department of Chemistry,Tsinghua University,Beijing 100084,China)

机构地区：[1]山东农业大学食品科学与工程学院,泰安271018 [2]山东省分析测试中心,济南250014 [3]清华大学化学系,北京100084

出　　处：《分析化学》2018年第12期1990-1996,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.21777089);山东省自然科学基金项目(No.ZR2018MB040);山东省重点研发项目(Nos.2017GSF17107;2018GSF117036);泰山学者建设工程项目(No.ts201712063)资助~~

摘　　要：以三聚氰胺/邻苯二甲醛共价有机骨架材料为固相萃取的吸附剂,建立了液相色谱-串联质谱法检测环境水样中磺胺类抗生素残留(磺胺嘧啶(SDZ)、磺胺噻唑(ST)、磺胺吡啶(SPD)、磺胺甲基嘧啶(SM1)、磺胺二甲嘧啶(SM2)、磺胺甲恶唑(SMX))。采用单因素优化法对影响萃取效果的重要因素进行优化,获得最佳条件为:洗脱液为8 mL甲醇,样品流速3 mL/min,样品溶液pH=4,穿透体积200 mL。液相色谱-串联质谱法检测萃取水样中磺胺类抗生素,在最佳条件下,检出限为0.05～0.36 ng/L,线性范围为0.25～1000 ng/L,日内标准偏差为0.6%～4.0%,日间标准偏差为2.1%～5.7%,样品加标回收率为82.5%～104.8%。本方法成功地应用于实际环境水样(饮用水、自来水、池塘水)中磺胺类化合物的检测,为快速、有效地检测环境水样中痕量磺胺类抗生素残留提供了良好选择。In this work,melamine/o-phthalaldehyde covalent organic framework was used as a novel trapping media in solid-phase extraction of sulfonamides at ultra-trace levels in real water samples.Six sulfonamides,including sulfadiazine(SDZ),sulfathiazole(ST),sulfapyridine(SPD),sulfamethyldiazine(SM1),sulfamethazine(SM2),sulfamethoxazole(SMX),were absorbed on the SPE cartridge.Important factors affecting extraction effect were optimized by single factor optimization method,and the optimized relevant parameters were as follows:eluent and its volume,8 mL MA;sample flow rate,3 mL/min;sample pH,pH=4 and sample volume,200 mL.Sulfonamide antibiotics were detected and quantified by liquid chromatography-tandem mass spectrometry.Low limits of detection(0.05-0.36 ng/L),wide linearity range(0.25-1000 ng/L),good repeatability and high recovery(82.5%-104.8%)for sulfonamides were obtained under the optimized conditions.The optimized method was used in the analysis of sulfonamides in real environmental water samples(drinking water,tap water and pool water)successfully.The novel COFs as a solid phase trapping material was a good choice for the rapid and effective analysis of sulfonamides at ultra trace levels in environmental water samples.

关 键 词：共价有机骨架材料 固相萃取 磺胺类抗生素 液相色谱-串联质谱 环境水样 

分 类 号：O657.63[理学—分析化学]