高效液相色谱法同时测定元胡止痛片中6种活性成分的含量
|
摘要
目的建立元胡止痛片(醋延胡索、白芷)中延胡索乙素、水合氧化前胡素、白当归素、欧前胡素、8-甲氧基异欧前胡内酯、异欧前胡素的含量测定方法。方法采用Agilent-ODS C18色谱柱(4.6mm×250 mm,5μm),流动相为(A)乙腈-(B)0.12%磷酸水溶液(pH=6.0),梯度洗脱(0～20min,25%A;20～40 min,25%～70%A;40～60 min,70%A);波长273 nm,流速1.0 mL·min~(-1);柱温40℃;进样体积15μL。结果延胡索乙素、水合氧化前胡素、白当归素、欧前胡素、8-甲氧基异欧前胡内酯、异欧前胡素进样量分别在测定浓度范围内与峰面积线性关系良好,平均加样回收率分别为95.5%、95.9%、92.8%、99.7%、96.7%、95.1%;RSD分别为3.9%、3.2%、3.0%、1.6%、4.2%、2.8%。结论本法结果准确,便于操作,可作为元胡止痛片的质量控制方法。
Objective To establish an HPLC method to determine the content of tetrahydropalmatine, oxypeucedanin hydrate, byakangelicin, imperatorin, cnidilin and isoimperatorin in Yuanhu Zhitong tablets. Methods The method was performed on an Agilent-ODS C18 colunm(4.6 mm×250 mm, 5 μm) in gradient elution manner with the mobile phase consisted of(A) acetonitrile-(B) 0.12% phosphoric acid water solution(pH = 6.0). The elution program was 0-20 min, 25% A; 20-40 min, 25%-70%A; 40-60 min, 70%A. The detection wavelength was 273 nm, the flow rate was 1.0 mL·min~(-1), and the column temperature was maintained at 40 ℃. Results The six constituents were well separated. Calibration curves showed good linearity. Average recoveries were 95.5%(RSD = 3.9%), 95.9%(RSD = 3.2%), 92.8%(RSD = 3.0%), 99.7%(RSD = 1.6%), 96.7%(RSD = 4.2%), and 95.1%(RSD = 2.8%), respectively. Conclusion The method is rapid, simple, and can be used for the quality control of Yuanhu Zhitong tablets.
Objective To establish an HPLC method to determine the content of tetrahydropalmatine, oxypeucedanin hydrate, byakangelicin, imperatorin, cnidilin and isoimperatorin in Yuanhu Zhitong tablets. Methods The method was performed on an Agilent-ODS C18 colunm(4.6 mm×250 mm, 5 μm) in gradient elution manner with the mobile phase consisted of(A) acetonitrile-(B) 0.12% phosphoric acid water solution(pH = 6.0). The elution program was 0-20 min, 25% A; 20-40 min, 25%-70%A; 40-60 min, 70%A. The detection wavelength was 273 nm, the flow rate was 1.0 mL·min~(-1), and the column temperature was maintained at 40 ℃. Results The six constituents were well separated. Calibration curves showed good linearity. Average recoveries were 95.5%(RSD = 3.9%), 95.9%(RSD = 3.2%), 92.8%(RSD = 3.0%), 99.7%(RSD = 1.6%), 96.7%(RSD = 4.2%), and 95.1%(RSD = 2.8%), respectively. Conclusion The method is rapid, simple, and can be used for the quality control of Yuanhu Zhitong tablets.
引文
[1]中国药典2015年版.一部[S]. 2015:602.
[2]夏文娟.元胡止痛片中有效成分含量与药理作用相关性研究[D].哈尔滨:黑龙江中医药大学,2011.
[3]赵亮.中药白芷有效成分提取、分离纯化及初步药理学研究及成药的质量控制研究[D].上海:第二军医大学,2013.
[4]孙绍欣,韩立炜,黄银峰,等.不同厂家元胡止痛片中延胡索乙素含有量比较[J].中成药,2012,34(1):180-182.
[5]杨芳,万里,杨荣平.一测多评法测定元胡止痛胶囊中欧前胡素、异欧前胡素、延胡索乙素含量[J].中国药房,2012,23(32):3046-2049.
[6]张婧,邹清河,刘辉,等. HPLC同时测定元胡止痛片中延胡索乙素与欧前胡素含量[J].中国药师,2012,15(12):1746-1748.
[7]路立峰,高源,汤志强.白芷质量控制的研究进展[J].中国药房,2017,28(15):2156-2160.
[8]毛志青,孟祥乐,李亚利,等. HPLC法测定白芷中4个香豆素类成分的含量[J].中国药师,2011,14(2):205-207.
[9]王云龙,李延雪,邵礼梅.元胡止痛片HPLC指纹图谱研究[J].中草药,2011,42(3):495-497.
[10]张虹,王麟,陈相涛,等.元胡炮制前后UPLC指纹图谱研究[J].中成药,2011,13(7):1903-1907.
[11]袁子民,赵强,贾天柱.白芷酒炖后化学成分变化[J].中成药,2016,38(11):2518-2520.
[12]张宇,李婷,杨建,等.白芷中有效成分的筛选、分析及对大鼠血管活性的影响[J].西北药学杂志,2015,30(1):37-42.
[13]肖炳燚,聂平,蒋秋桃.元胡止痛片UPLC特征图谱研究[J].中南药学,2014,12(4):294-296.
[14]陈东东,周萍,白钢钢,等.基于HPLC中药指纹图谱技术延胡索药材及其质量控制的探讨[J].中国中药杂志,2015,40(12):2470-2473.
[15]张剑萍.白芷香豆素类成分含量测定及药代动力学研究[D].苏州:苏州大学,2011.
[2]夏文娟.元胡止痛片中有效成分含量与药理作用相关性研究[D].哈尔滨:黑龙江中医药大学,2011.
[3]赵亮.中药白芷有效成分提取、分离纯化及初步药理学研究及成药的质量控制研究[D].上海:第二军医大学,2013.
[4]孙绍欣,韩立炜,黄银峰,等.不同厂家元胡止痛片中延胡索乙素含有量比较[J].中成药,2012,34(1):180-182.
[5]杨芳,万里,杨荣平.一测多评法测定元胡止痛胶囊中欧前胡素、异欧前胡素、延胡索乙素含量[J].中国药房,2012,23(32):3046-2049.
[6]张婧,邹清河,刘辉,等. HPLC同时测定元胡止痛片中延胡索乙素与欧前胡素含量[J].中国药师,2012,15(12):1746-1748.
[7]路立峰,高源,汤志强.白芷质量控制的研究进展[J].中国药房,2017,28(15):2156-2160.
[8]毛志青,孟祥乐,李亚利,等. HPLC法测定白芷中4个香豆素类成分的含量[J].中国药师,2011,14(2):205-207.
[9]王云龙,李延雪,邵礼梅.元胡止痛片HPLC指纹图谱研究[J].中草药,2011,42(3):495-497.
[10]张虹,王麟,陈相涛,等.元胡炮制前后UPLC指纹图谱研究[J].中成药,2011,13(7):1903-1907.
[11]袁子民,赵强,贾天柱.白芷酒炖后化学成分变化[J].中成药,2016,38(11):2518-2520.
[12]张宇,李婷,杨建,等.白芷中有效成分的筛选、分析及对大鼠血管活性的影响[J].西北药学杂志,2015,30(1):37-42.
[13]肖炳燚,聂平,蒋秋桃.元胡止痛片UPLC特征图谱研究[J].中南药学,2014,12(4):294-296.
[14]陈东东,周萍,白钢钢,等.基于HPLC中药指纹图谱技术延胡索药材及其质量控制的探讨[J].中国中药杂志,2015,40(12):2470-2473.
[15]张剑萍.白芷香豆素类成分含量测定及药代动力学研究[D].苏州:苏州大学,2011.