Simultaneous Determination of Eight Components in Xiaoer Anshen Bunao Granule by HPLC-MS

GAO Hou-ming; HU Zhao-liu; ZHENG Ping; LI Zhong-gui; ZHENG Lin; QIU Jing-yu; YI Tie-gang; ZHANG Shang-bin; CHEN Jian-ping

doi:10.13422/j.cnki.syfjx.20181911

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Simultaneous Determination of Eight Components in Xiaoer Anshen Bunao Granule by HPLC-MS

更新时间：2024-01-04

- Simultaneous Determination of Eight Components in Xiaoer Anshen Bunao Granule by HPLC-MS
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 24, Issue 19, Pages: 73-78(2018)
- 作者机构：
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20181911
  CLC： R286.0
- Published：2018
- 稿件说明：
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GAO Hou-ming, HU Zhao-liu, ZHENG Ping, et al. Simultaneous Determination of Eight Components in Xiaoer Anshen Bunao Granule by HPLC-MS[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(19): 73-78.
DOI：

GAO Hou-ming, HU Zhao-liu, ZHENG Ping, et al. Simultaneous Determination of Eight Components in Xiaoer Anshen Bunao Granule by HPLC-MS[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(19): 73-78. DOI： 10.13422/j.cnki.syfjx.20181911.

摘要

目的：建立高效液相色谱-串联质谱法同时测定小儿安神补脑颗粒中8个成分的含量测定方法。方法：采用Agilent TC-C18色谱柱（4.6 mm×250 mm，5 μm）；流动相乙腈（A）-10 mol·L-1乙酸铵（B）水溶液，梯度洗脱；进样量10 μL。质谱条件采用电喷雾离子源，正负离子同时检测，扫描方式为选择离子扫描模式。结果：甘草苷，毛蕊异黄酮葡萄糖苷，甘草酸铵，柚皮苷，3，6'-二芥子酰基蔗糖，橙皮苷，新橙皮苷和黄芪甲苷线性范围分别在0.019 5~2.5 mg·L-1（r=0.999 1），0.078 1~5 mg·L-1（r=0.999 2），0.078 1~5 mg·L-1（r=0.999 8），0.312 5~50 mg·L-1（r=0.999 9），0.019 5~2.5 mg·L-1（r=0.999 2），0.078 1~10 mg·L-1（r=0.999 0），0.312 5~20 mg·L-1（r=0.999 4），0.019 5~1.25 mg·L-1（r=0.999 0）；精密度、稳定性、重复性试验的RSD均<2%；平均回收率在95.07%~97.79%，RSD均<2%；甘草苷，毛蕊异黄酮葡萄糖苷，甘草酸铵，柚皮苷，3，6'-二芥子酰基蔗糖，橙皮苷，新橙皮苷和黄芪甲苷样品含量测定结果依次为187.5~188.1，330.0~331.0，312.1~319.5，1 509.0~1 510.2，172.2~173.0，180.0~181.0，639.0~639.8，37.5~38.2 μg·g-1。结论：该方法简单、准确、灵敏、重复性好，可用于小儿安神补脑颗粒的质量评价与控制。

Abstract

Objective: To establish a high performance liquid chromatography-mass spectrometry(HPLC-MS) method for simultaneously determining eight components in Xiaoer Anshen Bunao granule. Method: Agilent TC-C18(4.6 mm×250 mm

5 μm) column was adopted with acetonitrile-10 mol·L-1 ammonium acetate solution as the mobile phase for gradient elution

and the injection volume was 10 μL.Electrospray ionization (ESI) was used in both positive and negative modes

and the selected ion monitoring(SIM) were used for scanning. Result: Liquiritin

calycosin-7-O-β-D-glucoside

ammonium glycyrrhizinate

naringin

6'-disinapoyl sucrose

hesperidin

neohesperidin

astragaloside Ⅳ showed a good linearity in the ranges of 0.019 5-2.5 mg·L-1(r=0.999 1)

0.078 1-5 mg·L-1(r=0.999 2)

0.078 1-5 mg·L-1(r=0. 999 8)

0.390 6-50 mg·L-1(r=0.999 9)

0.019 5-2.5 mg·L-1(r=0.999 2)

0.078 1-10 mg·L-1(r=0.999 0)

0.312 5-20 mg·L-1(r=0.999 4)

0.019 5-1.25 mg·L-1(r=0.999 0)

respectively. Relative standard deviations (RSDs) of precision

stability and reproducibility were all less than 2.0%. The recoveries for the eight analytes were between 94.67% and 97.79%

with RSD less than 2.0%. The contents of liquiritin

calycosin-7-O-β-D-glucoside

ammonium glycyrrhizinate

naringin

6'-disinapoyl sucrose

hesperidin

neohesperidin

and astragaloside Ⅳ were 187.5-188.1

330.0-331.0

312.1-319.5

1 509.0-1 510.2

172.2-173.0

180.0-181.0

639.0-639.8

and 37.5-38.2 μg·g-1

respectively. Conclusion: This method is simple

accurate

sensitive and repeatable

which can be used for identification

quality evaluation of Xiaoer Anshen Bunao granule.

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