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

Analysis of Sulfonamides in Environmental Water Samples by High Performance Liquid Chromatography with Online Micro-solid-phase Extraction

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. 0μg/L,检出限为0. 3～0. 5μg/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。

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 1.0-50.0μgL,with their detection limits of 0.3-0.5μgL 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.