HPLC-CAD同时测定知母中芒果苷和知母皂苷B&#x02161;的含量<sup>&#x0002A;</sup>

南易, 郑伟, 马凤霞, 孙欣光, 赵阳, 张洁, 陈晓娟, 马百平

doi:10.16155/j.0254-1793.2021.01.13

药物分析杂志 >

2021 , Vol. 41 >Issue 1: 111 - 116

DOI: https://doi.org/10.16155/j.0254-1793.2021.01.13

标准研讨

HPLC-CAD同时测定知母中芒果苷和知母皂苷BⅡ的含量^*

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1.天津中医药大学,天津 300193;
2.军事医学研究院辐射医学研究所,北京 100850

第一作者 Tel：（010）66932247;E-mail：nanyi96@126.com

** Tel：（010）66930265;E-mail：mabaiping@sina.com

修回日期: 2020-11-25

网络出版日期: 2024-05-31

基金资助

* 国家自然基金面上项目（81373938）

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Simultaneous determination of mangiferin and timosaponin BⅡ of Anemarrhenae Rhizoma by HPLC-CAD^*

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1. Tianjin University of Traditional Chinese Medicine,Tianjin 300193,China;
2. Institute of Radiation Medicine,Academy of Military Medical Sciences,Beijing 100850,China

Revised date: 2020-11-25

Online published: 2024-05-31

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摘要

目的:建立HPLC-CAD 方法同时测定知母中芒果苷和知母皂苷BⅡ的含量。方法:采用Acclaim-C₁₈色谱柱（150 mm×4.6 mm,3 μm）,以乙腈（A）-0.2% 醋酸水溶液（B）为流动相,梯度洗脱（0~10 min,15%A → 21%A;10~12 min,21%A → 23%A,12~30 min,23%A → 25%A）,流速1.0 mL·min^-1,柱温30 ℃;电雾式检测器（CAD）参数：采集频率10 Hz,雾化温度55 ℃,滤波为5 s。结果:知母中芒果苷和知母皂苷BⅡ均具有良好的线性关系（r>0.999）,LOD 分别为0.43 ng 和1.20 ng,LOQ 分别为1.28 ng 和4.80 ng,精密度、重复性、24 h 稳定性试验的RSD 均小于3.0%,平均加样回收率分别为102.3% 和95.2%。11 批样品中芒果苷和知母皂苷BⅡ的含量范围分别为0.54%~1.69% 和3.27%~5.57%。结论:建立的HPLC-CAD 法可同时对知母中芒果苷和知母皂苷BⅡ进行含量测定,为知母药材和饮片的检测分析和质量控制提供了新的方法。

关键词： 知母; 芒果苷; 知母皂苷BⅡ; 双苯吡酮; 甾体皂苷; 高效液相色谱-电雾式检测器; 含量测定; 质量控制

本文引用格式

南易, 郑伟, 马凤霞, 孙欣光, 赵阳, 张洁, 陈晓娟, 马百平 . HPLC-CAD同时测定知母中芒果苷和知母皂苷BⅡ的含量^*[J]. 药物分析杂志, 2021 , 41(1) : 111 -116 . DOI: 10.16155/j.0254-1793.2021.01.13

Abstract

Objective: To establish an HPLC-CAD method for the determination of mangiferin and timosaponin BⅡ of Anemarrhenae Rhizoma. Methods: The analysis was performed on Acclaim-C₁₈ column（150 mm×4.6 mm,3 μm）．The mobile phase was acetonitrile（A） and 0.2% glacial acetic acid solution（B） by gradient elution （0-10 min,15%A → 21%A;10-12 min,21%A → 23%A;12-30 min,23%A → 25%A） at the flow rate 1.0 mL·min^-1．The column temperature was set at 30 ℃．The detector parameters were as follows：10 Hz for sampling rate,55 ℃ for the nebulizer temperature,and filter for 5 s. Results: The HPLC-CAD approach developed showed good linearity for mangiferin and timosaponin BⅡ,and the correlation coefficients（r） for calibration curves were both more than 0.999．The limit of detection（LOD） was 0.43 ng and 1.20 ng for mangiferin and timosaponin BⅡ,respectively．The limit of quantitation（LOQ） was found to be 1.28 ng and 4.80 ng,respectively．The RSDs of precision,repeatability,stability in 24 h were all less than 3.0%．The average recovery rate of mangiferin and timosaponin BⅡ was 102.3% and 95.2%,respectively．The contents of mangiferin and timosaponin BⅡ in 11 samples were 0.54%-1.69% and 3.27%-5.57% respectively. Conclusion: The established HPLC-CAD method can simultaneously determine mangiferin and timosaponin BⅡ in Anemarrhenae Rhizoma,which provides a new approach for the analysis and quality control of Anemarrhenae Rhizoma.

Key words： Anemarrhenae Rhizoma; mangiferin; timosaponin BⅡ; diphenylpyrrolidones; steroidal saponins; HPLC-CAD; content determination; quality control

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