目的 建立同时测定钩藤中绿原酸、异钩藤碱、钩藤碱、去氢毛钩藤碱、毛钩藤碱、喜果苷含量的方法,基于化学计量学分析,评价钩藤的质量。方法 采用高效液相色谱(HPLC),KinetexC18色谱柱(4.6 mm×100 mm,2.6 μm),以乙腈(A)-0.1%磷酸水(含0.5 g·L-11-丁基-3-甲基咪唑氯盐)(B)为流动相,梯度洗脱,流速:0.8 mL·min-1;检测波长327 nm(绿原酸)、246 nm(异钩藤碱、钩藤碱、去氢毛钩藤碱、毛钩藤碱和喜果苷);柱温:35 ℃;进样量:10 μL。结果 绿原酸、异钩藤碱、钩藤碱、去氢毛钩藤碱、毛钩藤碱和喜果苷分离良好,平均回收率分别为99.74%、103.25%、98.35%、99.45%、104.16%、97.98%。11批钩藤上述成分的含量测定结果分别为0.128 7～0.432 0、0.007 1～0.022 1、0.008 1～0.023 7、0.009 8～0.047 1、0.005 7～0.022 8、0.008 9～0.034 9 mg·g-1。化学计量学分析表明不同产地的钩藤质量存在一定差异。结论 建立的钩藤多指标含量测定方法简单、准确,可为钩藤药材质量综合评价提供新的参考方法。
Abstract
OBJECTIVE To establish a method for simultaneous determination of chlorogenic acid,isorhychophylline,rhynchophylline, hirsuteine, hirsutine, and vincosamide in uncariae ramulus cum uncis, and to evaluate its quality based on chemometric analysis. METHODS HPLC was used. The analysis was performed on a Kinetex C18 column(4.6 mm×100 mm,2.6 μm), with the mobile phase consisted of acetonitrile(A)-0.1% phosphoric acid water(containing 0.5 g·L-11-buty-3-methylimidazolium chloride)(B) in gradient elution mode. The flow rate was 0.8 mL·min-1, and the detection wavelength was set at 327 nm for chlorogenic acid) and 246 nm for isorhychophylline, rhynchophylline, hirsuteine, hirsutine and vincosamide. The column temperature was maintained at 35 ℃, and injection volume was 10 μL. RESULTS Chlorogenic acid,isorhychophylline, rhynchophylline,hirsuteine, hirsutine, and vincosamide were separated well, with the average recovery rates of 99.74%, 103.25%, 98.35%, 99.45%, 104.16% and 97.98%, respectively. The contents of chlorogenic acid,isorhychophylline, rhynchophylline,hirsuteine, hirsutine, and vincosamide in 11 batches samples from different habitats were 0.128 7-0.432 0, 0.007 1-0.022 1, 0.008 1-0.023 7, 0.009 8-0.047 1, 0.005 7-0.022 8 and 0.008 9-0.034 9 mg·g-1, respectively. Chemometric analysis showed that there were certain quality differences among the samples from different areas. CONCLUSION The method is simple and accurate. It can provide a new reference method for the comprehensive quality evaluation of uncariae ramulus cum uncis.
关键词
钩藤 /
多指标成分 /
含量测定 /
高效液相色谱法 /
化学计量学
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Key words
uncariae ramulus cum uncis /
muti-index component /
content determination /
HPLC /
chemometrics
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中图分类号：
R917
R282
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参考文献
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脚注
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基金
河南省科技厅工程技术研究中心建设项目资助(2020338);河南省中医专项课题重大专项资助(2019ZYZD08)
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