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

A Quantitative NMR Method to Analyze Vitamin B1,Vitamin B2,Nicotinamide and Calcium Pantothenate Contents in Compound Vitamin B Tablets

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（D_1）为1.0 s、脉冲宽度（P_1）为3.0μs、采样次数（NS）为500次.以对苯二甲醛为内标,其质子峰δ10.12（2H）为内标峰;溶剂为氘代二甲亚砜（DMSO-d_6）.定量峰的化学位移VB1选择δ9.60~9.90（~1H）,VB2选择δ11.36（~1H）,烟酰胺选择δ9.01（~1H）,泛酸钙选择δ0.78（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.

A quantitative 1H NMR method was established for analysis of contents ofvitamin B1, vitamin B2, nicotinamide and calcium pantothenate in Compound Vitamin BTablets. 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 forquantitative 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 thestandard curves obtained for the 4 components were close to theoretically predicted values.Calibration with vitamin B1 and calcium pantothenate reference substances yieldedcorrelation coefficients （r） above 0.999 and recovery ratio near 100%. Finally, the methodwas applied to 4 real samples, and the results suggested that it is simple to use, accurateand reliable.