反相离子对高效液相色谱法测定盐酸黄酮哌酯片的含量

RP - IP - HPLC Determination of Flavoxate Hydrochloride Tablets

目的:建立一种采用反相离子对高效液相色谱法测定盐酸黄酮哌酯片含量的方法。方法:用Shim-Pack vp-ODS柱(4.6mm×150mm,5μm),以0.05mol·L^(-1)磷酸二氢钾(含1％三乙胺,用磷酸调pH3.8)-0.0025mol·L^(-1)庚烷磷酸钠甲醇溶液(1:1.2)为流动相,流速1mL·min^(-1),UV检测波长241nm。柱温:室温,进样量20μL。结果:盐酸黄酮哌酯和前体杂质3-甲基黄酮-8-羧酸的保留时间分别为7.0min和5.0min,分离度为6.0,最低检测浓度分别为1.20μg·mL^(-1)和0.55μg·mL^(-1)。盐酸黄酮哌酯在0.119～0.834mg·mL^(-1)范围内呈良好的线性关系,r=0.9999。平均回收率(n=5)分别为99.04％(RSD=0.66％),99.36％(RSD=0.87％),99.64％(RSD=0.62％)。结论:本方法简便、快速、专属,结果准确可靠,能有效控制产品质量。

Objective: To establish a method of RP - IP - HPLC determination for flavoxate hydrochloride tablets. Methods: Employed Shim - Pack vp - ODS column (4. 6 mm ×150 mm, 5 μm) , 0. 05 mol · L-1 KH2PO4 (containing 1% triethylamine adjusted to pH 3. 8 with phosphoric acid) -0. 002 5 mol · L-1 sodium heptanesul-fonate methanol solution (1: 1. 2) as mobile phase (a flow rate of 1. 0 mL · min-1) , 241 nm as ultraviolet detec-tion wavelength, column temperature at room temperature and injection volume 20 μL. Results: The chromato-graphic peaks with a good resolution of 6. 0 at 7. 0 min and 5. 0 min resulted from flavoxate hydrochloride and pre -matter 3 - methylflavone - 8 - carboxylic acid, respectively. Their minimum detectable concentrations were re-spectively 1. 20 μg · mL-1 and 0. 55 μg · mL-1. The calibration curve of flavoxate hydrochloride was linear in the concentration range of 0. 119 -0. 834 mg · mL-1, r =0. 999 9. The average recovery rates (n =5) were 99. 04% (RSD=0. 66%), 99.36% (RSD=0. 87%) and 99. 64% (RSD=0.62%), respectively. Conclusion: The method is simple, rapid and specific with accurate and reliable results, which can be used to control the quality of products effectively.