高效液相色谱法测定益之康胶囊中总蒽醌(大黄素和大黄素甲醚)的含量
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摘要
建立益之康胶囊中总蒽醌含量测定的高效液相色谱法。采用HPLC测定益之康胶囊中2种蒽醌类成分大黄素和大黄素甲醚的含量;流动相为甲醇-0.1%磷酸溶液(75∶25,v/v),柱温30℃,流速1.0 m L/min,检测波长254 nm。大黄素和大黄素甲醚分别在0.054~0.65μg和0.022~0.27μg范围内呈良好的线性关系,相关系数分别为0.9999和0.9999,检出限分别为0.86μg/g和0.87μg/g,平均回收率分别为97.20%(RSD=2.26%)和99.96%(RSD=2.18%)。结论:该方法简便、准确、可靠。
Objective: To establish a High Performance Liquid Chromatography( HPLC) method for determining the totalanthraquinone in Yizhikang capsule.Methods: The contents of emodin and physcion were determined by a HPLC method.The emodin and physcion were separated on a Waters Sunfire C18 column( 250 mm × 4.6 mm,5 μm) using a mobile phase made up of methanol and 0.1% phosphoric acid solution( 75∶ 25,v/v) at a flow rate of 1.0 m L/min and detected by a UV detector at a wavelength of 254 nm.The column temperature was set at 30 ℃.Results: The response showed good linear relationship in the range of 54.09~649.05 μg/m L for emodin,22.11 ~ 265.31 μg/m L for physcion with all the coefficients of correlation( R2) =0.9999. The detection limits( LODs) were 0.86 μg/g for emodin,0.87 μg/g for physcion,respectively.The average recoveries of emodin and physcion were 97.20%( RSD = 2.26%) and 99.96%( RSD = 2.18%),respectively. Conclusions: This method is simple,accurate,reliable and reproducible and can be used for the quality control of yizhikang capsule.
Objective: To establish a High Performance Liquid Chromatography( HPLC) method for determining the totalanthraquinone in Yizhikang capsule.Methods: The contents of emodin and physcion were determined by a HPLC method.The emodin and physcion were separated on a Waters Sunfire C18 column( 250 mm × 4.6 mm,5 μm) using a mobile phase made up of methanol and 0.1% phosphoric acid solution( 75∶ 25,v/v) at a flow rate of 1.0 m L/min and detected by a UV detector at a wavelength of 254 nm.The column temperature was set at 30 ℃.Results: The response showed good linear relationship in the range of 54.09~649.05 μg/m L for emodin,22.11 ~ 265.31 μg/m L for physcion with all the coefficients of correlation( R2) =0.9999. The detection limits( LODs) were 0.86 μg/g for emodin,0.87 μg/g for physcion,respectively.The average recoveries of emodin and physcion were 97.20%( RSD = 2.26%) and 99.96%( RSD = 2.18%),respectively. Conclusions: This method is simple,accurate,reliable and reproducible and can be used for the quality control of yizhikang capsule.
引文
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[10]朱培芳,赵荣华,施扬宪.HPLC法同时测定何首乌中二苯乙烯苷和5种蒽醌类化合物的方法[J].中华中医药杂志,2012,27(2):463-465.
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[12]蔡丽芬,钟国跃,张倩,等.HPLC测定不同生长年限及采收期何首乌中二苯乙烯苷和蒽醌类成分的含量[J].中国中药杂志,2010,35(10):1221-1225.
[13]史辑,刘梓晗,王玲,等.HPLC测定不同产地巴戟天中5种茜草素型蒽醌的含量[J].中药材,2015,38(2):245-248.
[14]李樱红,汪瑾,胡磊,等.HPLC测定红曲黄酮片中总蒽醌的含量[J].中国现代应用药学,2012,29(12):1131-1133,1139.
[15]吴迪,袁海铭,曾宪仪,等.HPLC法测定大黄总蒽醌胶囊5种蒽醌苷元及5种游离蒽醌含量[J].江西中医药大学学报,2016,28(1):68-70.
[16]徐乾丽,茅向军,熊慧林.HPLC法测定六味安消胶囊中游离蒽醌、总蒽醌和结合蒽醌的含量[J].贵阳医学院学报,2010,35(6):578-580,583.
[17]戴作波,张建霞.HPLC法测定自制降脂胶囊中大黄蒽醌衍生物的含量[J].临床合理用药,2016,9(2A):95-96.
[18]韩燕全,洪燕,谢道俊,等.HPLC法同时测定黄蒲通窍胶囊中3种蒽醌类成分的总含量[J].云南中医中药杂志,2011,32(2):56-58.
[19]胡建华,陈文芝,徐超群,等.HPLC梯度洗脱测定痔康泰纳米粒中大黄蒽醌成分的总含量[J].华西药学杂志,2009,24(3):288-290.
[20]袁琦,杨洁,赵辉,等.HPLC测定一清胶囊中的5种大黄蒽醌衍生物[J].华西药学杂志,2014,29(4):430-432.
[2]王春英,张兰桐,袁志芳,等.何首乌醋酸乙酯提取部位与二苯乙烯苷的调血脂作用[J].中草药,2008,39(1):78-83.
[3]顾慧,吕圭源,陈素红,等.何首乌“补肝肾、益精血、强筋骨”功效相关的药理研究[J].世界科学技术-中医现代化,2008,10(2):58-62.
[4]楼招欢,吕圭源,俞静静.何首乌成分、药理及毒副作用相关的研究进展[J].浙江中医药大学学报,2014,38(4):495-500.
[5]梅雪,余刘勤,陈小云,等.何首乌化学成分和药理作用的研究进展[J].药物评价研究,2016,39(1):122-131.
[6]史国兵.炮制对何首乌中有效成分含量的影响[J].中国医院药学杂志,2003,23(2):95-97.
[7]施群,施淑琴.炮制对何首乌总蒽醌含量的变化研究[J].中华中医药学刊,2012,30(12):2770-2772.
[8]刘云娣,李得堂,任结梅,等.紫外分光光度法测定大承气冲剂中大黄总蒽醌的含量[J].中医药导报,2010,16(7):108-110.
[9]王玉宝.紫外分光光度法测定决明子中蒽醌类成分含量[J].中医药临床杂志,2013,25(8):730-732.
[10]朱培芳,赵荣华,施扬宪.HPLC法同时测定何首乌中二苯乙烯苷和5种蒽醌类化合物的方法[J].中华中医药杂志,2012,27(2):463-465.
[11]付卫华.HPLC法测定何首乌炮制过程中主要化学成分含量[J].亚太传统医药,2013,9(7):50-51.
[12]蔡丽芬,钟国跃,张倩,等.HPLC测定不同生长年限及采收期何首乌中二苯乙烯苷和蒽醌类成分的含量[J].中国中药杂志,2010,35(10):1221-1225.
[13]史辑,刘梓晗,王玲,等.HPLC测定不同产地巴戟天中5种茜草素型蒽醌的含量[J].中药材,2015,38(2):245-248.
[14]李樱红,汪瑾,胡磊,等.HPLC测定红曲黄酮片中总蒽醌的含量[J].中国现代应用药学,2012,29(12):1131-1133,1139.
[15]吴迪,袁海铭,曾宪仪,等.HPLC法测定大黄总蒽醌胶囊5种蒽醌苷元及5种游离蒽醌含量[J].江西中医药大学学报,2016,28(1):68-70.
[16]徐乾丽,茅向军,熊慧林.HPLC法测定六味安消胶囊中游离蒽醌、总蒽醌和结合蒽醌的含量[J].贵阳医学院学报,2010,35(6):578-580,583.
[17]戴作波,张建霞.HPLC法测定自制降脂胶囊中大黄蒽醌衍生物的含量[J].临床合理用药,2016,9(2A):95-96.
[18]韩燕全,洪燕,谢道俊,等.HPLC法同时测定黄蒲通窍胶囊中3种蒽醌类成分的总含量[J].云南中医中药杂志,2011,32(2):56-58.
[19]胡建华,陈文芝,徐超群,等.HPLC梯度洗脱测定痔康泰纳米粒中大黄蒽醌成分的总含量[J].华西药学杂志,2009,24(3):288-290.
[20]袁琦,杨洁,赵辉,等.HPLC测定一清胶囊中的5种大黄蒽醌衍生物[J].华西药学杂志,2014,29(4):430-432.