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通过血红素上羧基与端氨基聚乳酸上的氨基之间进行酰胺化反应,制得了血红素-聚乳酸分子。利用六氟异丙醇与端羧基反应生成六氟异丙醇酯,结合19F NMR峰面积积分的方法测定羧基含量,以荧光胺作为荧光试剂,采用荧光光谱法测定伯胺端基。进而,采用端基分析方法计算了血红素-聚乳酸的数均分子量,检测了血红素与聚乳酸1∶1和1∶2投料比(物质的量比)时的偶联反应。实验结果说明,利用二环己基碳二亚胺(DCC)脱水,N-羟基-苯并三氮唑(HOBt)催化,可以制备含血红素的生物降解高分子。关键词荧光胺;19F核磁共振;端基分析;偶联反应
The heme-polylactic acid molecule was obtained by amidation reaction between the carboxyl group on the heme and the amino group on the terminal amino polylactic acid. The hexafluoroisopropanol ester was synthesized by the reaction of hexafluoroisopropanol with carboxyl group and the content of carboxyl groups was determined by 19F NMR peak area integration. The primary amine end group was determined by fluorescence spectroscopy with fluorescent amine as fluorescent reagent. Furthermore, the number average molecular weight of heme-polylactic acid was calculated by end-group analysis, and the coupling reaction of heme and polylactic acid at the ratio of 1: 1 and 1: 2 (mass ratio) was tested. The experimental results show that heme-containing biodegradable polymer can be prepared by dehydration of dicyclohexylcarbodiimide (DCC) and HOBt catalyzed by N-hydroxy-benzotriazole (HOBt). Key words Fluorescein amine; 19F NMR; End group analysis; Coupling reaction