摘要
改进处方制备新工艺双氢青蒿素片,并建立双氢青蒿素片溶出度测定新方法,为修订标准提供参考。采用2015年版《中国药典》四部通则0931第二法测定新工艺及原工艺双氢青蒿素片的溶出度,溶出介质为0.1 mol·L^(-1)盐酸溶液250mL,转速为100 r·min^(-1),30 min取样。采用高效液相色谱法测定:Agilent Eclipse XDB-C_(18)色谱柱(4.6 mm×150 mm,5μm);流动相乙腈-水(40∶60);流速1.0 mL·min^(-1);柱温30℃;检测波长216 nm;进样体积100μL。双氢青蒿素检测线性范围为1.234 5～79.003 ng(r=1.000 0);定量限为0.308 6 ng,检测限为0.154 3 ng;精密度的RSD<1.0%;回收率98.09%～102.6%(RSD=1.8%,n=9)。在此条件下,3批新工艺双氢青蒿素片的溶出度分别为93.81%,92.61%,92.37%,1批原处方双氢青蒿素片的溶出度为32.67%。该方法重复性好、准确、可靠,能客观地反映双氢青蒿素片的溶出情况,为本品现行药品标准中溶出度项的修订提供了依据。另外,新工艺双氢青蒿素片的溶出度显著高于原处方双氢青蒿素片的溶出度,表明新的处方和工艺更合理。
New Dihydroartemisinin Tablets were prepared,and a new dissolution determination method for the tablets was established,which provides reference for revising the quality standard.The dissolution experiment adopted the paddle method with 0.1 mol·L^-1 hydrochloric acid solution 250 m L as the solvent,the rotating speed of 100 r·min^-1 and the sampling time of 30 min.HPLC was adopted to determine the dissolution of dihydroartemisinin.The determination was performed on Agilent Eclipse XDB-C18column with the mobile phase of acetonitrile-water(40∶60)at the flow rate of 1.0 m L·min^-1.The detection wavelength was set at 216 nm,and the column temperature was 30℃.The sample size was 100μL.The linear range of dihydroartemisinin were 1.234 5-79.003 ng(r=1.000 0).The limit of quantitation was 0.308 6 ng,and the limit of detection was 0.154 3 ng.RSDs of precision tests were all lower than 1.0%.The recoveries were 98.09%-102.6%(RSD 1.8%,n=9).The average dissolutions of dihydroartemisinin in 3 batches of samples were 93.81%,92.61%,92.37%,respectively.The determination method is highly reproducible,accurate and reliable,and can objectively reflect the dissolution of Dihydroartemisinin Tablets,and provide a basis for revising the dissolution test of the current quality standard.Based on the dissolution rate,new tablets are superior to original tablets.
作者
张东
仝燕
袁涛
王锦玉
杨岚
ZHANG Dong;TONG Yan;YUAN Tao;WANG Jin-yu;YANG Lan(institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Xinjiang Technical Institute of Physics and Chemistry,Chinese Academy of Sciences,Urumqi 830011,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2019年第6期1273-1277,共5页
China Journal of Chinese Materia Medica
基金
国家"重大新药创制"科技重大专项(2017ZX09101002-002-001)
中国中医科学院自主选题项目(ZZ10-002)
新疆理化技术研究所所长基金项目(2015RC015)
