核磁共振波谱法测定胆酸甲酯的含量  

NMRS Determination of Methyl Ester of Cholic Acid

作　　者：叶汝汉[1,2] 张怡 陈江韩[1,2] 柳亚玲[2] 陈泳[2] 潘文龙[2] 

机构地区：[1]广州法尔麦兰药物技术有限公司,广州510070 [2]中国广州分析测试中心广东省分析测试技术公共实验室,广州510070

出　　处：《理化检验（化学分册）》2016年第4期386-391,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：广东省科技计划项目(2012B040307002)

摘　　要：采用核磁共振波谱法测定胆酸甲酯的含量。以顺丁烯二酸为内标，氘代二甲基亚砜和重水为溶剂，测试温度为298K，脉冲宽度为8μs，弛豫时间为50S，扫描次数为16次。δ6．28为顺丁烯二酸的定量峰，δ3．79和δ0．59为胆酸甲酯的定量峰，以两个定量峰试验结果的平均值计算胆酸甲酯的含量。顺丁烯二酸与胆酸甲酯的定量峰不受其他信号干扰，顺丁烯二酸与胆酸甲酯的质量比在0．208-1．03范围内呈线性。胆酸甲酯的绝对含量测定结果为99．4％，测定值的相对标准偏差（n=6）为0．33％。NMRS was applied to the determination of methyl ester of cholic acid. Maleic acid was used as the internal standard. Deuterated dimethyl sulfoxide and deutoxide were used as solvents. The testing temperature taken was 298 K, the pulse width was 8/zs, the relaxation time was 50 s, and the number of scanning was 16. The proton signals at δ 3. 79 and δ 0. 59 for methyl ester of cholic acid, and at δ 6. 28 for maleic acid were selected for quantification. The content of methyl ester of cholie acid was obtained by calculating the average of test results of 2 quantitative peaks. Linearity range of mass ratio of maleic acid and methyl ester of cholic acid was found between 0. 208-1.03. The content of methyl ester of cholic acid found was 99.4% with RSD （n=6） of 0. 33%.

关 键 词：核磁共振波谱法 胆酸甲酯 含量 

分 类 号：O657.2[理学—分析化学]