Chullasat Kochaporn, Nurerk Piyaluk, Kanatharana Proespichaya, Kueseng Pamornrat, Sukchuay Thanyaporn, Bunkoed Opas
Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112, Thailand; Center of Excellence for Innovation in Chemistry, Department of Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112, Thailand.
School of Science, Walailak University, Thasala, Nakhon Si Thammarat 80161, Thailand.
Anal Chim Acta. 2017 Apr 8;961:59-66. doi: 10.1016/j.aca.2017.01.052. Epub 2017 Feb 1.
A hybrid monolith sorbent of polypyrrole-coated graphene oxide embedded in polyvinyl alcohol cryogel was prepared and used as an effective solid phase extraction sorbent for the determination of trace sulfonamides. The large surface areas with many adsorption sites of polypyrrole and graphene oxide facilitated the high adsorption of sulfonamides via hydrogen bonding, π-π and hydrophobic interactions. The high porosity of the polyvinyl alcohol cryogel helped to reduce the back pressure that occurs in a conventional packed solid phase extraction cartridge. The effecting parameters on the extraction efficiency including the type of sorbent, the polymerization time, desorption conditions, the sample pH, the sample volume, the sample flow rate, and ionic strength were investigated and optimized. Under the optimum conditions, the developed method provided a wide linear range from 0.20 to 100.0 μg L for sulfadiazine, sulfathiazole and sulfamerazine; and from 0.10 to 100 μg L for sulfamethazine, sulfamonomethoxine and sulfadimethoxine. The limits of detection were 0.20 μg L for sulfadiazine, sulfathiazole and sulfamerazine; and 0.10 μg L for sulfamethazine, sulfamonomethoxine and sulfadimethoxine. The developed hybrid monolith polypyrrole-coated graphene oxide embedded in the polyvinyl alcohol cryogel sorbent provided good recoveries in the range of 85.5-99.0% with RSDs of less than 5.0%. The sorbent offered a good reproducibility, was robust and can be reused at least 10 times. It was successfully applied for the extraction and enrichment of sulfonamides from normal and supplemented water samples.
制备了一种嵌入聚乙烯醇冷冻凝胶中的聚吡咯包覆氧化石墨烯混合整体吸附剂，并将其用作测定痕量磺胺类药物的有效固相萃取吸附剂。聚吡咯和氧化石墨烯具有大表面积和许多吸附位点，通过氢键、π-π相互作用和疏水相互作用促进了磺胺类药物的高吸附。聚乙烯醇冷冻凝胶的高孔隙率有助于降低传统填充固相萃取柱中出现的背压。研究并优化了影响萃取效率的参数，包括吸附剂类型、聚合时间、解吸条件、样品pH值、样品体积、样品流速和离子强度。在最佳条件下，所建立的方法对磺胺嘧啶、磺胺噻唑和磺胺甲基嘧啶的线性范围为0.20至100.0 μg/L；对磺胺二甲嘧啶、磺胺间甲氧嘧啶和磺胺二甲氧嘧啶的线性范围为0.10至100 μg/L。磺胺嘧啶、磺胺噻唑和磺胺甲基嘧啶的检测限为0.20 μg/L；磺胺二甲嘧啶、磺胺间甲氧嘧啶和磺胺二甲氧嘧啶的检测限为0.10 μg/L。所制备的嵌入聚乙烯醇冷冻凝胶吸附剂中的聚吡咯包覆氧化石墨烯混合整体吸附剂的回收率在85.5-99.0%范围内，相对标准偏差小于5.0%。该吸附剂具有良好的重现性，性能稳定，可重复使用至少10次。它已成功应用于从正常水样和加标水样中萃取和富集磺胺类药物。
