| 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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| 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） |
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| 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%～986%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 |
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| Analysis of Sulfonamides in Environmental Water Samples by High Performance Liquid Chromatography with Online Micro solid phase Extraction |
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| 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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