利用液相層析對兩磺胺藥物分子之辨識與鑑定   全文下載

Molecular Recognition and Identification of Sulfapyridine and Sulfadimethoxine by High Performance Liquid Chromatography with Molecularly Imprinted Polymer as the Stationary Phase

本研究以磺胺?啶作為模板分子，甲基丙烯酸作為功能性單體，在4°C低溫，進行自由基聚合反應。反應所得高分子材料，稱為分子模印高分子。此材料經真空乾燥之後，研磨為25~44 微米顆粒，填充管柱洗去模板分子，在高分子顆粒上可留下與模板分子形狀互補的孔洞，以作為高效率液相層析的固定相。利用顆粒上的模印孔洞，此固定相可以有效辨識兩磺胺藥物：磺胺?啶與磺胺二甲氧基嘧啶。本研究以磷酸緩衝液/ 乙氰（體積比3:2），作為移動相沖提液。實驗結果顯示，合成的高分子顆粒具備良好的分子模印辨識效果。兩磺胺藥物分子在管柱中滯留時間分別為8.24 與3.89 分鐘，分離因子為2.39；11 分鐘內可以完成樣品所需之分析。應用於市售錠劑之分析檢測，也可以得到良好之精確度與回收率。本研究並探討，合成分子模印高分子最佳化之條件與最佳移動相之組成，包含交聯單體的摩耳百分比、最適的反應溫度與功能性單體之使用等。分子模印高分子可以經由經濟便宜的材料、簡單合成步驟而具備良好辨識能力且樣品溶液不需經複雜之處理步驟。較之文獻利用氣相層析- 質譜儀、毛細管電泳、電化學分析與其他液相層析要方便並且快速的多。

Molecular imprinting technique is becoming an important tool for determining sulfonamides because of its simplicity and high separation efficiency. The creation of molecularly imprinted polymers (MIPs) for recognition of sulfapyridine and sulfadimethoxine is reported. Polymers were prepared using methacrylic acid (MAA) as the functional monomer and sulfapyridine as the template during imprinting. The recognition properties of the polymers were assessed by high performance liquid chromatography (HPLC) for their ability to retain the templates and analogous analytes. Retention time of sulfapyridine and sulfadimethoxine was approximately 8.24 and 3.89 min, respectively. In order to compare the chromatographic data from the stationary phase, both retention factor (k’) and separation factor (α) were given. The value of 2.39 for separation factor indicated that the MIP was able to recognize structurally subtle differences from the template molecule. Our results are discussed with regard to the amount of template, the compositions of the chromatographic mobile phase and the adsorption capacity.