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替考拉宁高效液相色谱手性固定相的制备研究
Preparation of Chiral Teicoplanin Stationary Phase in HPLC
【作者】 李倩;
【导师】 袁黎明;
【作者基本信息】 云南师范大学 , 分析化学, 2019, 硕士
【摘要】 本论文主要以替考拉宁为手性识别剂,采用键合的方法制备得到9种高效液相色谱手性固定相,并用于苯甘氨酸、对羟基苯甘氨酸的拆分。主要工作如下:(1)以4,4’-二苯基甲烷二异氰酸酯为键合臂制备替考拉宁手性固定相,并用对氯苯基异氰酸酯,间甲基苯基异氰酸酯衍生替考拉宁手性固定相得到其衍生物固定相。三种手性固定相均对苯甘氨酸、对羟基苯甘氨酸有一定的拆分能力。(2)以2,4-甲苯二异氰酸酯为键合臂制备替考拉宁手性固定相,并用对氯苯基异氰酸酯,间甲基苯基异氰酸酯衍生替考拉宁手性固定相得到其衍生物固定相。三种手性固定相均对苯甘氨酸、对羟基苯甘氨酸有拆分能力。(3)以1,6-己二异氰酸酯为键合臂制备替考拉宁手性固定相,并用对氯苯基异氰酸酯衍生替考拉宁手性固定相得到其衍生物固定相。两种手性固定相均对苯甘氨酸、对羟基苯甘氨酸有不同程度的拆分能力。(4)以3-异氰酸酯基丙基三乙氧基硅烷为键合臂制备替考拉宁固定相,这种手性固定相对苯甘氨酸、对羟基苯甘氨酸也均具有拆分能力。
【Abstract】 In this paper,nine chiral stationary phases of teicoplanin for high performance liquid chromatography were prepared to recognize phenylglycine and p-hydroxyphenylglycine.The main work is as follows:(1)Teicoplanin was bonded by 4,4’-diphenylmethane diisocyanate to amino propyl silica gel,and then its derivative was reacted further with p-chlorophenyl isocyanate and m-methylphenyl isocyanate,respectively.Three stationary phases have enantioselective resolution ability for phenylglycine and p-hydroxyphenylglycine in HPLC.(2)Teicoplanin was also bonded using 2,4-toluene diisocyanate to amino propyl silica gel,and its derivative was also reacted respectively with p-chlorophenyl isocyanate and m-methylphenyl isocyanate.Three stationary phases of HPLC can separate the recamates of phenylglycine and p-hydroxyphenylglycine.(3)With 1,6-hexadiisocyanate and p-chlorophenyl isocyanate,two teicoplanin chiral stationary phases were fabricated.Both chiral stationary phases were able to resolve phenylglycine and p-hydroxyphenylglycine.(4)Teicoplanin stationary phase was prepared by 3-isocyanate-propyl triethoxysilane as bonding arm.The optical resolutions of phenylglycine and p-hydroxyphenylglycine were obtained on the stationary phase.
【Key words】 Teicoplanin; Chiral stationary phase; High-performance liquid chromatography; Chiral separation;