Simultaneous Determination of Content of 10 Components in Fufang Daqingye Mixture by UPLC

LIN Lin; LIU Guang-zhen; GUO Dong-xiao; XU Li-hua; LIN Yong-qiang

doi:10.13422/j.cnki.syfjx.20180918

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Simultaneous Determination of Content of 10 Components in Fufang Daqingye Mixture by UPLC

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- Simultaneous Determination of Content of 10 Components in Fufang Daqingye Mixture by UPLC
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 24, Issue 12, Pages: 47-51(2018)
- 作者机构：
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20180918
  CLC： O657.72;R286.0
- Published：2018
- 稿件说明：
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LIN Lin, LIU Guang-zhen, GUO Dong-xiao, et al. Simultaneous Determination of Content of 10 Components in Fufang Daqingye Mixture by UPLC[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(12): 47-51.
DOI：

LIN Lin, LIU Guang-zhen, GUO Dong-xiao, et al. Simultaneous Determination of Content of 10 Components in Fufang Daqingye Mixture by UPLC[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(12): 47-51. DOI： 10.13422/j.cnki.syfjx.20180918.

摘要

目的：建立同时测定复方大青叶合剂中没食子酸，新绿原酸，绿原酸，隐绿原酸，异绿原酸A，异绿原酸B，紫花前胡苷，异绿原酸C，大黄酚和大黄素的含量测定方法。方法：采用Waters CORTECS-C18色谱柱（4.6 mm×150 mm，2.7 μm），甲醇（A）-0.4%甲酸溶液（B）为流动相，梯度洗脱（0~10 min，10%~3% A；10~25 min，3%~35% A；25~35 min，35%~36% A；35~55 min，36%~80% A），柱温和流速分别为30℃和0.3 mL·min-1，波长切换，0~10 min，290 nm；10~38 min，330 nm；38~55 min，250 nm。结果： 10种成分实现完全分离，并与其他成分均能达到良好的分离；没食子酸，新绿原酸，绿原酸，隐绿原酸，异绿原酸A，异绿原酸B，紫花前胡苷，异绿原酸C，大黄酚和大黄素分别在0.47～47.02，1.00～100.14，1.40～140.18，1.15～115.11，0.41～41.17，0.32～32.11，0.70～70.48，0.67～67.22，0.11～10.53，0.12～12.29 ng与色谱峰峰面积呈良好线性关系；平均回收率（n=6）分别为99.4%，99.7%，99.8%，99.7%，99.4%，99.3%，99.8%，99.4%，99.4%，99.3%；RSD分别为1.0%，0.6%，0.6%，0.6%，1.0%，0.9%，0.8%，0.9%，1.2%，1.0%。结论：该方法多种成分同时测定，操作简便，准确、重复性好，可用于复方大青叶合剂的质量控制。

Abstract

Objective: To develop a method for determining 10 components in Fufang Daqingye mixture. Method: The quantitative analysis was carried out on a column of Waters CORTECS-C18(4.6 mm×150 mm

2.7 μm) by UPLC-PDA

and eluted with a mobile phase of methanol (A)-0.4% formic acid solution (B) in a gradient mode (0-10 min

10%-3%A; 10-25 min

3%-35%A; 25-35 min

35%-36%A; 35-55 min

36%-80%A) under a flow rate of 0.3 mL·min-1 at 30℃. The detection wavelength was set at 290 nm in first 10 min

then changed to 330 nm between 10 and 38 min

and later changed to 250 nm between 38 and 55 min. Result: The linear ranges of gallic acid

neochlorogenic acid

chlorogenic acid

cyclohexanecarboxylic acid

isochlorogenic acid A

isochlorogenic acid B

nodakenin

isochlorogenic acid C

chrysophanol and emodin were 0.47-47.02

1.00-100.14

1.40-140.18

1.15-115.11

0.41-41.17

0.32-32.11

0.70-70.48

0.67-67.22

0.11-10.53

0.12-12.29 ng. The recoveries were 99.4%

99.7%

99.8%

99.7%

99.4%

99.3%

99.8%

99.4%

99.4% and 99.3%

respectively. The relative standard deviations were 1.0%

0.6%

1.0%

0.9%

0.8%

0.9%

1.2% and 1.0%

respectively (n=6). Conclusion: This method is simple

accurate

reproducible and convenient for the quality control over Fufang Daqingye mixture.

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