卡马西平片溶出度方法的改进研究及溶出行为的评价

目的: 改进卡马西平片溶出度检测方法并对不同样品进行溶出曲线评价。方法: 采用HPLC法,使用Kromasil 100-5C₁₈ Dimensions(250 mm×4.6 mm,5 μm)色谱柱,以0.051 8 mol·L^-1醋酸铵(冰醋酸调节pH至4.0)-甲醇(65:35)为流动相,流速1.0 mL·min^-1,检测波长为285 nm;溶出度试验采用桨法,以含0.2%十二烷基硫酸钠的pH 6.8磷酸缓冲液为溶出介质,转速为75 r·min^-1。结果: 在本文色谱条件下,卡马西平质量浓度在5.540~221.6 μg·mL^-1(r=1.000)检测范围内线性关系良好;低、中、高3种浓度的平均回收率分别为98.7%、100.0%和99.1%,RSD分别为0.78%、0.20%和0.94%,该色谱方法较好地对卡马西平溶出量进行了测定;溶出度方法较好地反映了不同厂家不同批次间卡马西平片溶出行为的差异。 结论: 所建立的色谱条件简单方便,提高了溶出量检测专属性和准确性,改善后的溶出方法较好地体现了片剂间的差异。

Objective: To improve the method for determination of dissolved carbamazepine tablets and evaluate the dissolution curves of different samples. Methods: The HPLC was used, and the separation was performed on a Kromasil 100-5C₁₈ Dimensions (250 mm×4.6 mm, 5μm) colum with the mobile phase consisted of 0.051 8 mol·L^-1 ammonium acetate (adjust pH to 4.0 by acetic acid)-methanol (65: 35) at a flow rate of 1.0 mL·min^-1. The detection wavelength was 285 nm. The paddle method was used for the dissolution test with pH 6.8 phosphate buffer containing 0.2% SDS as the medium and the rotation rate was set at 75 r·min^-1. Results: Under the chromatographic condition in this study, carbamazepine revealed a good linearity within the range of 5.540-221.6 μg·mL^-1(r=1.000). The average recoveries were 98.7% with RSD of 0.78%, 100.0% with RSD of 0.20%, 99.1% with RSD of 0.94% respectively at low, medium and high concentration,indicating that the chromatographic method detected well. The dissolution method was suitable, which showed differences of dissolutions among products of different lots and different manufacturers. Conclusion: The established HPLC method is simple, accurate and specific for determination of dissolved carbamazepine tablets. The improved dissolution method is more discriminating among different tablets than before.

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