高效液相色谱法测定复方苯硝那敏片中维生素B_6、苯巴比妥、马来酸氯苯那敏和硝西泮含量

Determination of vitaminB_6,phenobarbital,chlorphenamine maleate and diazepam in compound benxiaonamin tablets by HPLC

目的:建立HPLC同时测定复方苯硝那敏片中维生素B_6、苯巴比妥、马来酸氯苯那敏和硝西泮含量的方法。方法:色谱柱用十八烷基硅烷键合硅胶为固定相(150 mm×4.6 mm,4.6μm)。流动相A:乙腈-水-三乙胺(100:900:1,含0.01 mol/L庚烷磺酸钠,用冰醋酸调pH值3.5),流动相B:乙腈。洗脱程序:0～12 min,A 100%～70%;12～200 min,A 70%;流速:1 mL/min,检测波长260 nm。结果:维生素B_6、苯巴比妥、马来酸氯苯那敏和硝西泮的保留时间分别约为4.6、10.2、12.3和14.3 min,与各自相邻峰的分离度均大于1.5。以峰面积对进样量(μg)线性回归,维生素B_6回归方程:y=251.4x+2.403,线性范围:0.1684～2.021μg,r=0.9998;苯巴比妥回归方程:y=145.8x+1.612,线性范围:0.5108～6.130μg,r=0.999 9;马来酸氯苯那敏回归方程:y= 697.3x-7.252,线性范围:0.122 8～1.474μg,r=0.999 9;硝西泮回归方程:y=2767x+17.75,线性范围:0.04960～0.595 2μg,r=0.9998。维生素B_6、苯巴比妥、马来酸氯苯那敏和硝西泮回收率分别为100.1%、99.4%、99.3%和100.7%,RSD分别为0.18%、0.13%、0.47%和0.16%。结论:本方法精密度、准确度好,操作简便,可用于复方苯硝那敏片中维生素B_6、苯巴比妥、马来酸氯苯那敏和硝西泮含量测定。

Objective：To develop an HPLC quantitative method for the determination of vitaminB6, phenobarbital, chlorphenamine maleate and diazepam in compound benxiaonamin tablets. Methods： The chromatographic conditions include column C18 （150 mm ×4.6 mm, 4.6 um） ; mobile phase A： acetonitrile-water-triethylamine（ 100 ： 900 ： 1 ,contain 0.01 mol / L Sodium Heptane, adjusted to pH 3.5 by acetic acid） ; mobile phase B ： acetonitrile, gradient elution ： 0 - 12 min, A ： 100% - 70% , 12 - 20 min, A ： 70% . The flow rate was 1 mL/min and monitored at 260 nm. Results： The retention time of vitaminB6,phenobarbital,chlorphenamine maleate and diazepam were 4.6 min, 10.2 min, 12.3 min and 14.3 min respectively. The regress equation for VitaminB6 was y = 251.4x ＋ 2. 403, r = 0. 999 8, and the linear range was 0.168 4 - 2. 021 ug, phenobarbital y = 145.8x ＋ 1. 612, r = 0. 999 9 , and the linear range was 0.510 8 - 6.130 ug; chlorphenamine maleate y = 697.3x -7. 252, r = 0. 999 9, and the linear range was 0. 122 8 - 1. 474 ug, diazepam y = 276 7x ＋ 17.75, r = 0. 999 8 and the linear range was 0. 049 60 - 0. 595 2ug . The average recovery of vitaminB6, phenobarbital, chlorphenamine maleate and diazepam were 100.1% ,99.4% ,99.3 % and 100.7% ; and RSD were 0.18% , 0.13% , 0.47% and 0.16% respectively. Conclusion： The method was sensiteve,time-saving and accurate.