摘要
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.
出处
《药学实践杂志》
CAS
2008年第4期286-289,共4页
Journal of Pharmaceutical Practice