HPLC法测定二(2-噻吩基)乙醇酸东莨菪酯和2,2-二噻吩基乙醇酸甲酯的含量  

Determination of Scopine-2,2-dithienyl Glycolate and Methyl 2,2-dithienyl Glycolate by HPLC Method

作　　者：陈红[1] 李来生[1] 方奕珊[1] 张杨[1] 

机构地区：[1]南昌大学分析测试中心,江西南昌330047

出　　处：《南昌大学学报（理科版）》2011年第5期447-449,463,共4页Journal of Nanchang University(Natural Science)

基　　金：国家自然科学基金资助项目(21165012);江西省自然科学基金资助项目(2010GZH0089)

摘　　要：建立了测定二(2-噻吩基)乙醇酸东莨菪酯和2,2-二噻吩基乙醇酸甲酯的含量的HPLC方法。采用μBondapakTMC18液相色谱柱(3.9mm i.d.×250mm,10μm),以乙腈/戊烷磺酸钠溶液(35/65,v/v,pH=7.0)为流动相,流速设定为0.8mL.min-1,检测波长为215nm时,实现了这两种酯的良好分离分析。二(2-噻吩基)乙醇酸东莨菪酯的线性范围为1.52～194μg.mL-1,r=0.999 6;2,2-二噻吩基乙醇酸甲酯的线性范围为1.61～206μg.mL-1,r=0.999 6。平均加标回收率及RSD分别为94.43%(RSD 5.66%)和96.21%(RSD 4.39%)。本方法灵敏度高、选择性好、操作简单,可方便地用于监测噻托溴铵合成反应的过程,也适用于检测噻托溴铵中间体含量。An HPLC（HPLC） method of determination of scopine-2,2-dithienyl glycolate and methyl 2,2-dithienyl glycolate in reaction solution was developed.Baseline separaton was achieved on a μBondpakTM C18（4.6 mm i.d.×250 mm,10 μm） by using the acetonitrile/sodium pentanesulfonate buffer（35：65,v/v,pH=7.0） as mobile phase at a flow rate of 0.8 mL·min-1.The detection wavelength was set at 215 nm.The linear ranges and the correlation coefficient of methyl 2,2-dithienyl glycolate and scopine-2,2-dithienyl glycolate were between 1.52~194 μg·mL-1（r=0.999 6） and 1.61~206 μg·mL-1（r=0.999 6）,respectiviely.The average recoveries were 94.43% with RSD 5.66% for the scopine ester and 96.21% with RSD 4.39% for the methyl ester.The method was found to be sensitive,selective and simple for the monitoring of the synthetic process of tiotropium bromide and the determination of the related intermediates as well.

关 键 词：高效液相色谱法 噻托溴铵 二(2-噻吩基)乙醇酸东莨菪酯 2 2-二噻吩基乙醇酸甲酯 

分 类 号：O657.7[理学—分析化学]