中药制剂含量均匀度的测定方法初探
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摘要
目的:以自制的银黄片为材料,分析高效液相色谱检测含量均匀度评价结果,分析采用红外线光谱分析最小二乘法检测不同处理方法的含量预测效果。方法:取金银花提取物,45%,w/w,黄苓提取物,9.5%,w/w,预胶化淀粉,44.0%,w/w,硬脂酸镁,1.38%,称取四种物质,进行等量递增混合,压制成片。取药品溶解,按照《中国药典》二部附录推荐的含量测定方法,采用高效液相色谱检测计算有效成分。采用最小二乘法红外线光谱预测成分,与色谱法检测真实值对比,计算误差均方根。结果:红外线光谱分析不同处理方法不同成分含量预测误差均方根多组间对比差异有统计学意义(P<0.05),经典的MSC方法四种成分误差均方根均最低,差异有统计学意义(P<0.05)。高效液相色谱检测第一批、第二批、第三批、第四批金银花提取物均值±标准差变异指数在5%,一致性较好。结论:高效液相色谱是测定中药制剂含量均匀度的首选方法,检测精度高;红外线光谱分析具有一定的含量均匀度分析潜力,在控制误差的前提下能够较好的反映含量均匀度。
Objective:To analyze the results of content uniformity evaluation by high performance liquid chromatography(HPLC) with silver yellow tablets made by ourselves.Methods:Flos Lonicerae extract from Flos Lonicerae was extracted from Flos Lonicerae at 45 W/w,Huangling extract 9.5 w/w,pre-gelatinized starch 44.0 w/w,magnesium stearate 1.38 g.Compacted tablets,dissolute the drugs,the active components were measured by HPLC in accordance with the method recommended in the appendix to part II of the Chinese Pharmacopoeia.The infrared spectrum of square method was used to predict the composition,and the true value was compared with that of chromatographic detection.Results:There were significant differences in the prediction errors of different components in different methods of infrared spectrum analysis(P<0.05),and the classical MSC method had the lowest root-mean-square error of the four components.The difference was statistically significant(P<0.05).The mean ±standard deviation variation index of 4 th batches of Flos Lonicerae extract was 5,with good consistency.Conclusion:High performance liquid chromatography is the first choice to determine the content uniformity of traditional Chinese medicine preparations.The infrared spectrum analysis has a certain potential for content uniformity analysis,which can reflect the content uniformity better under the premise of controlling the error.
Objective:To analyze the results of content uniformity evaluation by high performance liquid chromatography(HPLC) with silver yellow tablets made by ourselves.Methods:Flos Lonicerae extract from Flos Lonicerae was extracted from Flos Lonicerae at 45 W/w,Huangling extract 9.5 w/w,pre-gelatinized starch 44.0 w/w,magnesium stearate 1.38 g.Compacted tablets,dissolute the drugs,the active components were measured by HPLC in accordance with the method recommended in the appendix to part II of the Chinese Pharmacopoeia.The infrared spectrum of square method was used to predict the composition,and the true value was compared with that of chromatographic detection.Results:There were significant differences in the prediction errors of different components in different methods of infrared spectrum analysis(P<0.05),and the classical MSC method had the lowest root-mean-square error of the four components.The difference was statistically significant(P<0.05).The mean ±standard deviation variation index of 4 th batches of Flos Lonicerae extract was 5,with good consistency.Conclusion:High performance liquid chromatography is the first choice to determine the content uniformity of traditional Chinese medicine preparations.The infrared spectrum analysis has a certain potential for content uniformity analysis,which can reflect the content uniformity better under the premise of controlling the error.
引文
[1]国家药典委员会.国家药品标准工作手册[M].4版,北京:中国医药科技出版社,2013.
[2]Dale L M,Thewis A,Boudry C,et al.Hyperspectral imaging applications in agriculture and agro-food product quality and safety control:A review[J].Applied Spectroscopy Reviews,2013,48(2):142-159.
[3]刘占京.论中药质量控制与评价模式的创新与发展[J].中医临床研究,2014,6(1):127-128.
[4]肖宏华,孙磊,金红宇,等.5种升麻中有机酸、色原酮和三萜皂苷的薄层色谱指纹图谱分析[J].药物分析杂志,2014,34(3):547-553.
[5]尤献民,邹桂欣,邸子真.波长切换高效液相色谱法同时测定化胃舒颗粒中4种有效成分的含量[J].中国药业,2014,23(4):35-37.
[6]韩丽,张芳,张定堃,等.中药制剂含量均匀度的测定方法初探[J].中药,2014,45(15):2125-2131.
[7]许佳楠,邓剑壕,冯豆,等.中药固体制剂均匀性问题分析[J].中国实验方剂学杂志,2017,23(4):228-234.
[8]董海彦.连蒲双清片含量均匀度的考察[J].华西药学杂志,2014,29(4):478-479.
[9]丁海樱,金叶,刘雪松.中药粉末混合过程近红外在线检测研究[J].中国药学杂志,2013,48(14):1151-1156.
[10]李强,杜思邈,张忠亮,等.中药指纹图谱技术进展及未来发展方向展望[J].中草药,2013,44(22):3095-3104.
[2]Dale L M,Thewis A,Boudry C,et al.Hyperspectral imaging applications in agriculture and agro-food product quality and safety control:A review[J].Applied Spectroscopy Reviews,2013,48(2):142-159.
[3]刘占京.论中药质量控制与评价模式的创新与发展[J].中医临床研究,2014,6(1):127-128.
[4]肖宏华,孙磊,金红宇,等.5种升麻中有机酸、色原酮和三萜皂苷的薄层色谱指纹图谱分析[J].药物分析杂志,2014,34(3):547-553.
[5]尤献民,邹桂欣,邸子真.波长切换高效液相色谱法同时测定化胃舒颗粒中4种有效成分的含量[J].中国药业,2014,23(4):35-37.
[6]韩丽,张芳,张定堃,等.中药制剂含量均匀度的测定方法初探[J].中药,2014,45(15):2125-2131.
[7]许佳楠,邓剑壕,冯豆,等.中药固体制剂均匀性问题分析[J].中国实验方剂学杂志,2017,23(4):228-234.
[8]董海彦.连蒲双清片含量均匀度的考察[J].华西药学杂志,2014,29(4):478-479.
[9]丁海樱,金叶,刘雪松.中药粉末混合过程近红外在线检测研究[J].中国药学杂志,2013,48(14):1151-1156.
[10]李强,杜思邈,张忠亮,等.中药指纹图谱技术进展及未来发展方向展望[J].中草药,2013,44(22):3095-3104.