核磁共振波谱法测定片剂中维生素B_1的含量  

Determination of Vitamin B_1 in Tablets by NMR

作　　者：鲁瑞娟[1] 吴崇荣[1] 方萍[1] 

机构地区：[1]绍兴文理学院分析测试中心,绍兴312000

出　　处：《理化检验（化学分册）》2016年第3期323-327,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：绍兴文理学院科研资助项目(2015LG1003)

摘　　要：采用Bruker AVANCEⅢ400MHz核磁共振波谱仪,溶剂为D2O,内标为顺丁烯二酸,脉冲序列为zg30,谱宽为20.55ppm,采样时间为3.98s,采样温度为298K,延迟时间为20s,采样次数为16次,在此条件下采集样品1 H-NMR谱。样品中维生素B1与内标的质量比与NMR谱图中相应的定量峰面积比呈线性关系。此方法应用于片剂中维生素B1的含量测定,测得维生素B1、复合维生素B片剂中维生素B1的含量分别为11.33%,2.54%,测定值的相对标准偏差（n≥5）均小于4%;加标回收率为在97.4%～101%之间。^1H-NMR spectra were obtained with a Bruker AVANCEⅢ 400 MHz spectrometer at 298 K with maleic acid as intemal standard and D2O as solvent.For each sample,16 times of sampling were recorded under the following conditions：the pulse sequence of zg30,acquisition time of 3.98 s,spectra width of 20.55 ppm and delayed time of 20 s.A linear relationship was found between the mass ratio of vitamin B1 with the internal standard and the corresponding ratio of quantitative peak areas.The proposed method was used to determine vitamin B1 in tablets,and the contents of vitamin B1 in vitamin B1 tablets and vitamin B complex tablets were 11.33% and2.54%,respectively,with RSDs（n≥5）less than 4%.Recovery rates obtained by standard addition method were in the range of 97.4%-101%.

关 键 词：核磁共振波谱法 维生素B1 片剂 

分 类 号：O657.3[理学—分析化学]