定量核磁共振法同时测定复合维生素B片中B1、B2、烟酰胺和泛酸钙

doi:10.11938/cjmr20160309

摘要/Abstract

摘要：

建立了同时测定复合维生素B片中4种有效成分——维生素B1（VB1）、维生素B2（VB2）、烟酰胺和泛酸钙的定量核磁共振氢谱（¹H qNMR）方法．选择延迟时间（D₁）为1.0 s、脉冲宽度（P₁）为3.0 μs、采样次数（NS）为500次．以对苯二甲醛为内标，其质子峰δ 10.12（2H）为内标峰；溶剂为氘代二甲亚砜（DMSO-d₆）．定量峰的化学位移VB1选择δ 9.60~9.90（1H），VB2选择δ 11.36（1H），烟酰胺选择δ 9.01（1H），泛酸钙选择δ 0.78（12H）．通过标定VB1和泛酸钙对照品的纯度，测定各成分的零截距标准曲线斜率与理论值相符，说明可以直接用绝对定量公式计算其含量．测定各成分的回收率均接近100%，且重复性很好．结果表明该方法准确度高、结果可靠，可用于复合维生素B片中VB1、VB2、烟酰胺和泛酸钙含量的测定．

关键词: 定量核磁共振氢谱(¹H qNMR), 复合维生素B片, 维生素B1(VB1), 维生素B2(VB2), 烟酰胺, 泛酸钙

Abstract:

A quantitative ¹H NMR method was established for analysis of contents of vitamin B1, vitamin B2, nicotinamide and calcium pantothenate in Compound Vitamin B Tablets. The experimental settings were as following: delay time (D₁) 1.0 s, pulse width (P₁) 3.0 μs, number of sampling (NS) 500 times, 1,4-benzenedialdehyde peak at δ 10.12 (2H) as the internal standard, and deuterated DMSO-d₆ as the solvent. The peaks for quantitative analysis were: vitamin B1 at δ 9.60~9.90 (1H), vitamin B2 at δ 11.36 (1H), nicotinamide at δ 9.01 (1H) and calcium pantothenate at δ 0.78 (12H). The slopes of the standard curves obtained for the 4 components were close to theoretically predicted values. Calibration with vitamin B1 and calcium pantothenate reference substances yielded correlation coefficients (r) above 0.999 and recovery ratio near 100%. Finally, the method was applied to 4 real samples, and the results suggested that it is simple to use, accurate and reliable.

Key words: quantitative ¹H NMR, Compound Vitamin B Tablets, vitamin B1 (VB1), vitamin B2 (VB2), nicotinamide, calcium pantothenate

中图分类号:

O482.53
R917

郭强胜, 刘明珂, 禹珊, 沈婷婷, 宋巍, 许旭. 定量核磁共振法同时测定复合维生素B片中B1、B2、烟酰胺和泛酸钙[J]. 波谱学杂志, 2016, 33(3): 442-451.

GUO Qiang-sheng, LIU Ming-ke, YU Shan, SHEN Ting-ting, SONG Wei, XU Xu. A Quantitative NMR Method to Analyze Vitamin B1, Vitamin B2, Nicotinamide and Calcium Pantothenate Contents in Compound Vitamin B Tablets[J]. Chinese Journal of Magnetic Resonance, 2016, 33(3): 442-451.

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