固相萃取-定量核磁共振波谱法测定双黄连胶囊中的绿原酸

doi:10.5246/jcps.2020.04.021

中国药学(英文版)

• 【研究论文】 • 下一篇

固相萃取-定量核磁共振波谱法测定双黄连胶囊中的绿原酸

刘晓婷, 徐静娜, 肖坤, 郭强胜, 许旭^*

上海应用技术大学化学与环境工程学院, 上海 201418

收稿日期:2020-01-12 修回日期:2020-02-20 出版日期:2020-04-30 发布日期:2020-03-15
通讯作者: Tel.: +86-21-60873372, E-mail: xuxu3426@sina.com
基金资助:
National Natural Science Foundation of China (Grant No. 31671928) and Natural Science Foundation of Shanghai (Grant No. 15ZR1440800).

Determination of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule using quantitative nuclear magnetic resonance spectroscopy in combination with solid phase extraction

Xiaoting Liu, Jingna Xu, Kun Xiao, Qiangsheng Guo, Xu Xu^*

School of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 201418, China

Received:2020-01-12 Revised:2020-02-20 Online:2020-04-30 Published:2020-03-15
Contact: Tel.: +86-21-60873372, E-mail: xuxu3426@sina.com
Supported by:
National Natural Science Foundation of China (Grant No. 31671928) and Natural Science Foundation of Shanghai (Grant No. 15ZR1440800).

摘要/Abstract

摘要：

建立了固相萃取(SPE)-定量核磁共振波谱(qNMR)测定双黄连胶囊中绿原酸含量的方法。绿原酸是双黄连胶囊处方中金银花提取物的有效成分。样品用纯水在室温条件下超声提取,以HC-C₁₈型SPE柱对提取液进行富集净化后,用qNMR测定绿原酸的含量。考察了超声时间、SPE样品前处理条件以及定量核磁共振实验条件对结果的影响。选择氘代二甲基亚砜为溶剂,标定后的对苯二甲醛作为内标。选择脉冲宽度P1 = 14.1 µs,延迟时间d1 = 1 s,扫描次数NS = 512为qNMR定量绿原酸的实验条件。绿原酸的定量峰为δ6.138–6.182 (H-8’, d, 1H)。结果显示,所建方法的日内精密度的RSD为1.2%,日间精密度RSD为1.5%,绿原酸与对苯二甲醛峰面积比与质量比的零截距标准曲线线性相关系数为0.9999,且斜率与理论值相符。该法测定绿原酸的LOD为0.0017 mg/g; LOQ为0.079 mg/g。包括样品经SPE预处理过程的绿原酸的回收率为100.2%~103.2%。实际测定双黄连胶囊中的绿原酸的含量为9.68~10.35 mg/g。

关键词: 定量核磁共振波谱法, 固相萃取, 绿原酸, 双黄连胶囊

Abstract:

The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy (qNMR) in combination with solid phase extraction (SPE). As the capsule’s main active component, chlorogenic acid comes from the extraction of Chinese herb medicine Flos Lonicerae. The chlorogenic acid in capsule was ultrasonically extracted at room temperature using pure water as solvent. The extracting solution was enriched and cleaned using HC-C₁₈ SPE cartridge. The effect of ultrasonic extraction, sample pretreatment conditions via SPE and qNMR experimental conditions were investigated. The qNMR experiment conditions were selected using deuterated DMSO as solvent, calibrated 1,4-phthalaldehyde as internal standard, and P1 (pulse width) = 14.4 μs, d1 (pulse delay time) = 1 s, NS (number of scan) = 512. The ¹H NMR peaks of δ 6.138–6.182 (H-8’, d, 1H) of chlorogenic acid was chosen as the quantitativepeaks. Method validation was performed, including precision (the intra-day RSD = 1.2% and the inter-day RSD = 1.5%), linearity (correlation coefficient r>0.9999), LOD (0.0017 mg/g) and LOQ (0.079 mg/g). The recovery of the SPE-qNMR was within the range of 100.2%–103.2%. The result showed that the method was stable, accurate and reliabile. Determined by the method, the chlorogenic acid in a real Shuanghuanglian capsule was within the range of 9.68–10.35 mg/g.

Key words: Quantitative nuclear magnetic resonance spectroscopy, Solid phase extraction, Chlorogenic acid, Shuanghuanglian capsule

中图分类号:

R917

Supporting:

刘晓婷, 徐静娜, 肖坤, 郭强胜, 许旭. 固相萃取-定量核磁共振波谱法测定双黄连胶囊中的绿原酸[J]. 中国药学(英文版), DOI: 10.5246/jcps.2020.04.021.

Xiaoting Liu, Jingna Xu, Kun Xiao, Qiangsheng Guo, Xu Xu. Determination of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule using quantitative nuclear magnetic resonance spectroscopy in combination with solid phase extraction[J]. Journal of Chinese Pharmaceutical Sciences, DOI: 10.5246/jcps.2020.04.021.

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固相萃取-定量核磁共振波谱法测定双黄连胶囊中的绿原酸

Determination of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule using quantitative nuclear magnetic resonance spectroscopy in combination with solid phase extraction

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