国产盐酸氯哌丁片含量与含量均匀度研究

Study on Content and Content Uniformity of Domestic Cloperastine Hydrochloride Tablets

目的:建立高效液相色谱法研究国产盐酸氯哌丁片的含量与含量均匀度质量状况。方法:采用Inertsil ODS-3(4.6mm×100 mm,3μm)色谱柱,以甲醇-0.1 mol·L-1磷酸二氢钾溶液-高氯酸(60∶40∶0.16)为流动相,检测波长为222 nm,进样量为10μL。结果:盐酸氯哌丁在20.02~200.2μg·m L-1浓度范围内线性关系良好(r=0.9993),两家企业样品平均回收率分别为100.2%(RSD=1.0%,n=9)和99.5%(RSD=0.8%,n=9)。106批次国产盐酸氯哌丁片的含量在82.7%~97.5%之间,均值为88.0%。89.6%的样品含量测定值超出标准规定的限度(90.0%~110.0%)。106批次国产盐酸氯哌丁片含量均匀度A+2.2S值在8.60~27.30之间,均值为21.04,96.2%的样品A+2.2S值>15.0。结论:该方法专属性强,可准确测定盐酸氯哌丁片的含量与含量均匀度。国产盐酸氯哌丁片的含量与含量均匀度质量状况较差。

Objective： A high performance liquid chromatography（HPLC） method was established to study the content and uniformity of domestic cloperastine hydrochloride tablets. Methods： A Inertsil ODS-3（4. 6 mm × 100 mm,3 μm） column was used with methanol-0. 1 mol·L-1 potassium dihydrogen phosphate solution-perchloric acid（60∶ 40： 0. 16） as the mobile phase,the detection wavelength was222 nm,the sample volume was 10 μL. Results： Cloperastine hydrochloride had a good linear relationship within the range of 20. 02 ~200. 2 μg·m L-1（r = 0. 9993）. The average recovery of two enterprise were 100. 2%（RSD = 1. 0%,n = 9） and 99. 5%（RSD = 0. 8%,n= 9）,respectively. The contents of 106 batches of domestic cloperastine hydrochloride tablets were in the range of 82. 7% ~ 97. 5%,and the average content was 88. 0%. The contents of 89. 6% domestic cloperastine hydrochloride tablets exceeds the limit（90. 0% ~110. 0%） specified in the standard. The value of A ＋ 2. 2 S of the 106 batches of domestic cloperastine hydrochloride tablets were in the range of 8. 60 ~ 27. 30,and the average value was 21. 04,the value of A ＋ 2. 2 S of 96. 2% samples greater than 15. 0. Conclusion： The method is specific,and can accurately determine the content and content uniformity of cloperastine hydrochloride tablets. The content and content uniformity of domestic cloperastine hydrochloride tablets were poor.