Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
J Chromatogr A. 2020 Nov 8;1631:461576. doi: 10.1016/j.chroma.2020.461576. Epub 2020 Sep 21.
A cryogel-based semi-interpenetrating polymer network (Cryo-SIPN) was prepared in which conductive polymers such as polyaniline (PANI) and polypyrrole (PPy) were formed within the super porous network of acrylic acid cryogel. For completion of cryo-polymerization, all the constituent solutions were severely mixed and placed into the plastic straws and kept at -20°C and then the synthesized cyrogels were cut into the 1-cm length and freeze dried after washing with water. The Cryo-SIPN polymeric composite was applied in micro solid phase extraction (µSPE) of some selected antibiotic residues from various samples. The µSPE method combined with a high performance liquid chromatography-ultraviolet (HPLC-UV) system allowed trace quantification of antibiotic residues in the honey and water samples while the significant variables were optimized using a central composite design (CCD) to find optimum conditions. The method performance was satisfactory with recovery ranges from 70.0 to 109%. The limits of detection (S/N = 3) and quantification (S/N = 10) for all samples were within the 17-50 μg kg and 47-140 μg kg range, respectively. The relative standard deviation was less than 10 % for antibiotics in the foodstuff and water samples. The validated Cryo-SIPN-µSPE in conjunction with HPLC-UV, proved to be versatile, efficient and robust while its capability toward the trace determination of drugs residues in real-life samples is demonstrated in this work.
一种基于 cryogel 的半互穿聚合物网络（Cryo-SIPN）被制备，其中导电聚合物如聚苯胺（PANI）和聚吡咯（PPy）在丙烯酸 cryogel 的超多孔网络内形成。为了完成 cryo-polymerization，所有的组成溶液都被剧烈混合并放入塑料吸管中，并保持在-20°C，然后将合成的 cryogels 切成 1 厘米长，并在用水洗涤后进行冷冻干燥。Cryo-SIPN 聚合物复合材料被应用于从各种样品中微固相萃取（µSPE）一些选定的抗生素残留。µSPE 方法与高效液相色谱-紫外（HPLC-UV）系统相结合，允许在蜂蜜和水样中痕量定量抗生素残留，而显著变量则使用中心复合设计（CCD）进行优化，以找到最佳条件。该方法的性能令人满意，回收率范围为 70.0 至 109%。所有样品的检测限（S/N=3）和定量限（S/N=10）均在 17-50 μg kg 和 47-140 μg kg 范围内。在食品和水样中的抗生素的相对标准偏差小于 10%。经过验证的 Cryo-SIPN-µSPE 与 HPLC-UV 结合使用，证明是多功能、高效和稳健的，同时证明了其在实际样品中痕量药物残留测定的能力。
