盐酸替扎尼定片溶出度方法的研究与改进

Research and Improvement of the Detection Method of Dissolution for Tizanidine Hydrochloride Tablets

目的改进盐酸替扎尼定片溶出度方法。方法统一溶出度方法为桨法,以盐酸溶液900 ml为溶出介质,转速为50 r/min;检测方法由原来的紫外分光光度法改为高效液相色谱法,色谱柱为C_（18）（5μm,4.6 mm×250 mm）,流动相为1-戊烷磺酸钠缓冲溶液（取1-戊烷磺酸钠3.5 g,溶于1000 ml水中,用12%磷酸溶液或氢氧化钠试液调节p H至3.0±0.05）-乙腈（80∶20）,流速为1.0 ml/min,检测波长为230 nm,35℃,进样量为20μl。比较两种方法测定的样品累积溶出度。结果盐酸替扎尼定检测质量浓度线性范围为0.5 022~5.0 225μg/ml（r=1.0 000）,平均回收率为99.4%,相对标准偏差为0.3%;样品的溶出时间由原来的30 min缩短至15 min。改进方法测定的盐酸替扎尼定片的累积溶出率高于原方法。结论改进方法提高了盐酸替扎尼定片溶出度检测的专属性和准确性,较好地体现了片剂间的差异。

Objective To improve the detection method of dissolution for Tizanidine Hydrochloride Tablets.Methods The paddle method was used as uniform method in the dissolution experiment,and 900 ml of hydrochloricacid solution was used as solvent with 50 r/min rotating speed. The determination method changed from ultraviolet spectrophotometry（ UV） to high performance liquid chromatography（ HPLC）. The chromatographic column was C_（18）（ 5 μm,4. 6 mm × 250 mm）; mobile phase consisted of 1-pentane sulfonic acid sodium salt buffer（ 3. 5 g 1-pentane sulfonic acid sodium salt was put into 1000 ml of water,and the p H value was adjusted to 3. 0 ± 0. 05 using 12% phosphoric acid or sodium hydroxide solution） and methyl cyanides（ 80∶ 20）; the flow rate was 1. 0 ml/min; the detection wavelength was set at 230 nm; the column temperature was 35℃,and the injection volume was 20 μl. The cumulative dissolution rates of the two detection methods were compared. Results The linear range of Tizanidine hydrochloride in detecting mass concentration were 0. 5 022-5. 0 225 μg/ml（ r = 1. 0 000） with 99. 4% of average recovery（ RSD = 0. 3%）. The dissolution time for the samples decreased to 15 min from the previous 30 min. The cumulative dissolution rate by improved method was higher than that by the original method for detecting Tizanidine Hydrochloride Tablets. Conclusion The method improves the specificity and accuracy of dissolution detection for Tizanidine Hydrochloride Tablets,and it may well show the distinction among different tablets.