高效液相色谱法测定当归芍药散不同极性部位中阿魏酸和芍药苷的含量
|
摘要
目的建立当归芍药散不同极性部位中阿魏酸和芍药苷的含量测定方法。方法采用高效液相色谱(HPLC)法测定当归芍药散不同极性部位中阿魏酸和芍药苷的含量,色谱柱为Kromasil 100-5-C18柱(4.6 mm×250.0 mm),流动相为甲醇∶0.2%磷酸溶液,梯度洗脱,流速1 mL/min,阿魏酸、芍药苷的检测波长分别为320,230 nm,进样量10μL,柱温30℃。结果阿魏酸和芍药苷的回归方程分别为Y=3.53×10~4X-4.83×10~2(r=0.999 0),Y=1.50×10~4X-2.51×10~4(r=0.999 9),线性范围分别为6.076～303.800μg/mL和7.448～372.400μg/mL;方法学考察中精密度、稳定性和重复性均符合要求,加样回收率的RSD分别为1.2%和1.1%。含量测定结果显示,除醇提物的水相部分未检出阿魏酸外,其他部分中均存在阿魏酸和芍药苷,且水煎液中阿魏酸、芍药苷含量均最高。结论该法简便、准确、分离效果好,可用于当归芍药散不同极性部位中阿魏酸、芍药苷的含量测定。
Objective To establish a content determination method for ferulic acid and paeoniflorin of different polar parts in Danggui Shaoyao San(当归芍药散).Methods HPLC was used with Kromasil 100-5-C18 column(4.6 mm×250.0 mm).The mobile phase was methanol ∶ 0.2% phosphoric acid solution with gradient elution.The flow rate was 1.0 mL/min,the detection wavelength of ferulic acid and paeoniflorin was 320 nm and 230 nm,respectively.The column temperature was 30 ℃,and sample size was 10 μL.Results The regression equations of ferulic acid and paeoniflorin were Y = 3.53×10~4 X-4.83×10~2(r=0.999 0) and Y=1.50×10~4 X-2.51×10~4(r=0.999 9),respectively.The linearity ranged from 6.076 to 303.800 μg/mL for ferulic acid,and from 7.448 to 372.400 μg/mL for paeoniflorin.The precision,stability and repeatability of methodological investigation meet the requirements.The RSD of sample recovery rate was 1.2% and 1.1%,respectively.The results of content determination showed that ferulic acid and paeoniflorin existed in other parts except in the aqueous phase of methanol extract,and the content of ferulic acid and paeoniflorin in water decoction was the highest.Conclusion The method is simple and accurate,with good separating effect.It can be used for content determination of ferulic acid and paeoniflorin of different polar parts in Danggui Shaoyao San.
Objective To establish a content determination method for ferulic acid and paeoniflorin of different polar parts in Danggui Shaoyao San(当归芍药散).Methods HPLC was used with Kromasil 100-5-C18 column(4.6 mm×250.0 mm).The mobile phase was methanol ∶ 0.2% phosphoric acid solution with gradient elution.The flow rate was 1.0 mL/min,the detection wavelength of ferulic acid and paeoniflorin was 320 nm and 230 nm,respectively.The column temperature was 30 ℃,and sample size was 10 μL.Results The regression equations of ferulic acid and paeoniflorin were Y = 3.53×10~4 X-4.83×10~2(r=0.999 0) and Y=1.50×10~4 X-2.51×10~4(r=0.999 9),respectively.The linearity ranged from 6.076 to 303.800 μg/mL for ferulic acid,and from 7.448 to 372.400 μg/mL for paeoniflorin.The precision,stability and repeatability of methodological investigation meet the requirements.The RSD of sample recovery rate was 1.2% and 1.1%,respectively.The results of content determination showed that ferulic acid and paeoniflorin existed in other parts except in the aqueous phase of methanol extract,and the content of ferulic acid and paeoniflorin in water decoction was the highest.Conclusion The method is simple and accurate,with good separating effect.It can be used for content determination of ferulic acid and paeoniflorin of different polar parts in Danggui Shaoyao San.
引文
[1]许成平.当归芍药散的临床研究进展[J].中国民族民间医药,2016,25(2):27-28.
[2]苗裕.当归芍药散在妇科病中的应用[J].河南中医,2015,35(3):459-460.
[3]曾宇,江滨,马世平,等.DPPH自由基清除法筛选当归芍药散抗氧化活性有效部位[J].广东药学院学报,2013,29(2):138-141.
[4]曾宇.当归芍药散抗衰老活性的药效学和药代学研究[D].广州:广州中医药大学,2013.
[5]马世平,詹莹,瞿融.当归芍药散的抗氧化作用研究[J].中药药理与临床,2001,17(3):1-3.
[6]尚玮玮,乔善义.当归芍药散研究概况[J].中国中药杂志,2006,31(8):630-633.
[7]杜星海.当归芍药散中芍药苷水提工艺考察研究[J].海峡药学,2012,24(4):29-31.
[8]陈春水,庞晓华.RP-HPLC法测定当归芍药散中芍药苷的含量[J].中国医药导报,2008,5(13):30-31.
[9]曾宇,杜迎翔,马世平.反相高效液相色谱法测定当归芍药散中阿魏酸和芍药苷的含量[J].中国药科大学学报,2004,35(4):51-53.
[10]贺晓艳,宋秋月,郑丹,等.HPLC法测定当归芍药散中芍药苷、白芍苷、阿魏酸、洋川内酯I的含量[J].亚太传统医药,2011,7(7):36-39.
[11]宋欣,陶春蕾,孟广东,等.高效液相-二极管阵列法检测当归芍药散中主要化学成分[J].安徽中医学院学报,2012,31(1):65-68.
[12]倪文澎,钱平,周琴妹,等.RP-HPLC法同时测定养生丸中芍药苷和阿魏酸的含量[J].中国药师,2010,13(8):1114-1116.
[13]毛晓敏,张小波,陈小清,等.HPLC同时测定十二乌鸡白凤丸中芍药苷、阿魏酸和丹皮酚含量[J].中成药,2008,30(5):678-681.
[14]李成义,祝永甲,王明伟,等.熏硫对商品当归不同药用部位阿魏酸含量的影响[J].甘肃中医学院学报,2013,30(3):20-23.
[15]刘俊,宋欣,王满媛,等.不同提取方法测定当归芍药散中芍药苷和阿魏酸含量的比较研究[J].亚太传统医药,2010,6(3):20-22.
[16]胡虒尧,周瑜,陶春蕾,等.当归芍药散HPLC-DAD指纹图谱峰来源分析[J].中国药科大学学报,2014,45(2):205.
[17]于宁,姜雯,帕依曼·亥米提,等.高效液相色谱法同时测定香青兰不同部位中5种化学成分的含量[J].中国药学杂志,2016,51(7):583-587.
[2]苗裕.当归芍药散在妇科病中的应用[J].河南中医,2015,35(3):459-460.
[3]曾宇,江滨,马世平,等.DPPH自由基清除法筛选当归芍药散抗氧化活性有效部位[J].广东药学院学报,2013,29(2):138-141.
[4]曾宇.当归芍药散抗衰老活性的药效学和药代学研究[D].广州:广州中医药大学,2013.
[5]马世平,詹莹,瞿融.当归芍药散的抗氧化作用研究[J].中药药理与临床,2001,17(3):1-3.
[6]尚玮玮,乔善义.当归芍药散研究概况[J].中国中药杂志,2006,31(8):630-633.
[7]杜星海.当归芍药散中芍药苷水提工艺考察研究[J].海峡药学,2012,24(4):29-31.
[8]陈春水,庞晓华.RP-HPLC法测定当归芍药散中芍药苷的含量[J].中国医药导报,2008,5(13):30-31.
[9]曾宇,杜迎翔,马世平.反相高效液相色谱法测定当归芍药散中阿魏酸和芍药苷的含量[J].中国药科大学学报,2004,35(4):51-53.
[10]贺晓艳,宋秋月,郑丹,等.HPLC法测定当归芍药散中芍药苷、白芍苷、阿魏酸、洋川内酯I的含量[J].亚太传统医药,2011,7(7):36-39.
[11]宋欣,陶春蕾,孟广东,等.高效液相-二极管阵列法检测当归芍药散中主要化学成分[J].安徽中医学院学报,2012,31(1):65-68.
[12]倪文澎,钱平,周琴妹,等.RP-HPLC法同时测定养生丸中芍药苷和阿魏酸的含量[J].中国药师,2010,13(8):1114-1116.
[13]毛晓敏,张小波,陈小清,等.HPLC同时测定十二乌鸡白凤丸中芍药苷、阿魏酸和丹皮酚含量[J].中成药,2008,30(5):678-681.
[14]李成义,祝永甲,王明伟,等.熏硫对商品当归不同药用部位阿魏酸含量的影响[J].甘肃中医学院学报,2013,30(3):20-23.
[15]刘俊,宋欣,王满媛,等.不同提取方法测定当归芍药散中芍药苷和阿魏酸含量的比较研究[J].亚太传统医药,2010,6(3):20-22.
[16]胡虒尧,周瑜,陶春蕾,等.当归芍药散HPLC-DAD指纹图谱峰来源分析[J].中国药科大学学报,2014,45(2):205.
[17]于宁,姜雯,帕依曼·亥米提,等.高效液相色谱法同时测定香青兰不同部位中5种化学成分的含量[J].中国药学杂志,2016,51(7):583-587.