高效液相色谱法测定乙酰乌头碱片含量及含量均匀度
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摘要
目的建立测定乙酰乌头碱片含量及含量均匀度的高效液相色谱法。方法色谱柱为Waters Bridge C18柱(250 mm×4. 6 mm,5μm),流动相为0. 1%碳酸氢铵溶液-乙腈(60∶40,V∶V),检测波长为232 nm,流速为1. 0 m L/min,进样量为20μL。结果乙酰乌头碱质量浓度在6. 0～60. 2μg/m L范围内与峰面积线性关系良好(r=0. 999 8);平均回收率为96. 91%,RSD为0. 58%(n=9); 3批样品的平均含量分别为100. 21%,99. 14%,99. 72%,含量均匀度(A+2. 2 S)分别为12. 23,8. 61,9. 32。结论该方法简便准确,重复性好,专属性强,可用作乙酰乌头碱片的质量控制。
Objective To establish an HPLC method for the determination of content and content uniformity of acetylaconitine in Acetylaconitine Tablets. Methods The chromatographic column was Waters Bridge C18 column( 250 mm × 4. 6 mm,5 μm),the mobile phase was 0. 1% ammonium bicarbonate solution-acetonitrile( 60 ∶ 40,V ∶ V),the detection wavelength was 232 nm,the flow rate was1. 0 m L/min and the sample size was 20 μL. Results Acetylacidine showed good linear relationship with peak area in the range of6. 0-60. 2 μg/m L( r = 0. 999 8),the average recovery was 96. 91% and RSD was 0. 58%( n = 9). The average contents of three batches of samples were 100. 21%,99. 14% and 99. 72%,the content uniformity( A + 2. 2 S) of three batches of samples was 12. 23,8. 61 and 9. 32,respectively. Conclusion The method is simple,accurate,reproducible and specific,which is suitable for the quality control of Acetylaconitine Tablets.
Objective To establish an HPLC method for the determination of content and content uniformity of acetylaconitine in Acetylaconitine Tablets. Methods The chromatographic column was Waters Bridge C18 column( 250 mm × 4. 6 mm,5 μm),the mobile phase was 0. 1% ammonium bicarbonate solution-acetonitrile( 60 ∶ 40,V ∶ V),the detection wavelength was 232 nm,the flow rate was1. 0 m L/min and the sample size was 20 μL. Results Acetylacidine showed good linear relationship with peak area in the range of6. 0-60. 2 μg/m L( r = 0. 999 8),the average recovery was 96. 91% and RSD was 0. 58%( n = 9). The average contents of three batches of samples were 100. 21%,99. 14% and 99. 72%,the content uniformity( A + 2. 2 S) of three batches of samples was 12. 23,8. 61 and 9. 32,respectively. Conclusion The method is simple,accurate,reproducible and specific,which is suitable for the quality control of Acetylaconitine Tablets.
引文
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[2]姚婉霞,陈夏平,张艳丽.三乙酰乌头碱镇痛作用及机制的初步研究[J].宁夏医学杂志,2014,36(5):388-390.
[3]王毓杰,曾陈娟,姚.铁棒锤及其炮制品中二萜生物碱化学成分研究[J].中草药,2010,41(3):347-351.
[4] WS-10001-(HD-0299)-2002.国家药品化学药品地方标准上升国家标准[S].
[5]国家药典委员会.中华人民共和国药典(四部)[M].北京:中国医药科技出版社,2015:通则0941.
[6]马新焕,郭敏,乔莉,等.甘肃不同地域伏毛铁棒锤中乌头碱及3-乙酰乌头碱的含量分析[J].西部中医药,2016,29(8):16-17.