手性分离_手性拆分_手性衍生试剂_1氮杂双环[2

柱前衍生高效液相色谱法分离分析1氮杂双环[2, 2, 2]辛3基胺对映异构体

http://www.100md.com 《分析化学》 2006年第10期

手性分离,手性拆分,手性衍生试剂,1氮杂双环[2,2,2]辛3基胺,高效液相色谱,,手性分离，手性拆分，手性衍生试剂，1氮杂双环[2,2,2]辛3基胺，高效液相色谱,柱前衍生高效液相

     摘要 1氮杂双环[2,2,2]辛3基胺是制备5羟色胺拮抗剂药物盐酸帕洛诺司琼等的重要中间体,手性帕洛诺司琼可以通过中间体的手性分离来制备。用柱前衍生化反相高效液相色谱法对1氮杂双环[2,2,2]辛3基胺对映体进行分离并建立了检测方法。结果表明，用2,3,4,6四O乙酰基βD葡萄糖异硫氰酸酯(GITC)为柱前手性衍生化试剂，C18柱(300 mm×4.6 mm, 5 μm)为色谱柱，可将1氮杂双环[2,2,2]辛3基胺对映体分离，其他色谱条件：流动相组成为[甲醇乙腈0.01 mol/L四丁基溴化铵(20∶10∶75， V/V)](三乙胺)01%(冰醋酸)0.15%，流速0.7 mL/min，检测波长为266 nm。在选择的测定条件下，衍生后的两非对映异构体分离度达4以上。

    关键词手性分离，手性拆分，手性衍生试剂，1氮杂双环[2,2,2]辛3基胺，高效液相色谱

    Enantiomeric Resolution and Quantitative Determination of (R/S)1Azabicyclo [2, 2, 2]octan3amine by Precolumn Derivatization High Performance Liquid Chromatography

    Deng Jie, Li Zhiliang, Xiao Yumei, Chen Xiaoyong*1,3, Liu xueguo,Deng Xianglin, Liu Qiping, Zhou Surong

    1(College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044)

    2(State Key Laboratory of Chemo/Biosensing and Chemometrics, Changsha 410082)

    3(Centre for Analytical Technology, Renben Institute of Pharmacy, Chongqing 400041)

    Abstract 1Azabicyclo[2,2,2]octan3amine is an important intermediate for the preparation of 5Hydroxytryptamine 3antagonist palonosetron hydrochloride. Chiral palonosetron can be synthesized by the enantioseparation of intermediates. A high performance liquid chromatographic method for the separation of 1azabicyclo[2,2,2]octan3amine has been developed. The results show that the enantiomers can be separated with 2,3,4,6tetraoacetylβDglucopyranosyl isothiocyanate(GITC) as the derivatization reagent and a column of C18(300 mm×4.6 mm, 5 μm). Other chromatographic conditions are mobile phase consisting of [methanolacetonitrile0.01 mol/L tetrabutylamine bromine (20∶10∶75 ......

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