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在线微固相萃取/高效液相色谱联用分析环境水样中磺胺类药物
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作者单位
周婵媛,罗军,王壹,严伟,聂胜强 贵阳学院化学与材料工程学院 
基金项目:贵州省教育厅青年科技人才成长项目(黔教合KY字[2018]293,黔教合KY字[2017]243);贵阳市科技局贵阳学院专项(GYU-KYZ[2018]03-08);贵州省一流大学专业建设项目(2017158134);贵州省科技合作计划(黔科合LH字[2015]7304)
中文摘要:通过酸化法制备氧化海泡石(O-Sep)材料,将其填充于自制PEEK微柱中,建立了O-Sep在线微固相萃取/高效液相色谱联用分析方法(O-Sep/μ-SPE/HPLC)对环境水样中3种磺胺类药物进行检测。研究了O-Sep微柱的结构与萃取性能,O-Sep微固相萃取柱对磺胺对甲氧嘧啶(SMD)、磺胺多辛(SDX)和磺胺苯吡唑(SPP)均有较好的富集效果,10 mg O-Sep固相萃取材料对SMD、SDX、SPP的饱和萃取容量分别为203.2、150.3、102.1 ng。方法用于SMD、SDX、SPP的检测,其线性范围为1.0~50.0 μg/L,检出限为0.3~0.5 μg/L,相对标准偏差(RSD)不大于5.0%。将所建分析方法应用于自来水、河水和雨水中此3种磺胺类药物(SAs)的分析,3种样品的加标回收率分别为79.5%~98.3%、74.3%~986%和70.2%~98.7%,RSD为1.4%~7.6%。该方法操作简便、灵敏、准确,在环境样品中痕量磺胺类药物的分析方面具有良好的应用前景。
中文关键词:磺胺类药物  氧化海泡石  在线微固相萃取  高效液相色谱
 
Analysis of Sulfonamides in Environmental Water Samples by High Performance Liquid Chromatography with Online Micro solid phase Extraction
Abstract:A novel method of high performance liquid chromatography coupled with oxidized sepiolite(O-Sep) based solid phase extraction(SPE) was developed for the analysis of sulfonamides in environmental water samples.The O-Sep was successfully synthesized by acid treatment,then packed into a homemade PEEK micro column,which had a high adsorption capacity towards sulfameter(SMD),sufladoxine(SDX) and sulfaphenazole(SPP),and the corresponding saturated extraction amounts of 10 mg O-Sep were 203.2,150.3 and 102.1 ng,respectively.The calibration curves of SMD,SDX and SPP showed good linear relationships in the range of 1.0-50.0 μg/L,with their detection limits of 0.3-0.5 μg/L and relative standard deviations(RSDs) not more than 5.0%.The method was applied in the simultaneous analysis of three analytes with satisfactory recoveries,which were 79.5%-98.3% for tap water,74.3%-98.6% for river water and 70.2%-98.7% for rain water with RSD of 1.4%-7.6%.This method was simple,sensitive and accurate,and showed a great potential in the determination of trace sulfonamides in environmental samples.
Key Words:sulfonamides  oxidized sepiolite  online μ-SPE  high performance liquid chromatography(HPLC)
引用本文:周婵媛,罗军,王壹,严伟,聂胜强.在线微固相萃取/高效液相色谱联用分析环境水样中磺胺类药物[J].分析测试学报,2018,37(12):1451-1456.
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