文章摘要
白术多指标成分含量测定方法优化
Optimization of Determination Method for Multi-indicator Content of Atractylodes Macrocephala Rhizoma
投稿时间:2019-12-19  修订日期:2020-05-26
DOI:
中文关键词: 白术  高效液相  多指标含量测定  方法优化  
英文关键词: Atractylodes macrocephala Rhizoma  HPLC  Multi-index content determination  Method optimization  
基金项目:浙江省公益技术研究计划项目(LGC20H280002),国家重点研发计划—中药饮片质量识别关键技术研究(2018YFC1707001),中华中医药学会青年人才托举工程项目(QNRC2-C12)
作者单位E-mail
王丽敏 杭州市中医院
浙江中医药大学中药炮制技术研究中心 
wlm19900730@163.com 
杜伟锋* 浙江中医药大学中药炮制技术研究中心 duweifeng_200158@sohu.com 
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中文摘要:
      目的:通过对白术含量测定方法优化研究,建立一种简单高效准确的白术多指标成分含量测定的方法。方法:采用HPLC-DAD测定白术中白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ和苍术酮四个指标成分,色谱条件:流动相为0.1%磷酸(A)和乙腈(B);流速:1.0ml/min;进样量10μl;色谱柱:ZORBAX Eclipse XDB-C18 Analytical 4.6×250 mm 5-Micron;梯度洗脱程序:0-8 min,60%B,8-16 min,60%B-75%B,16-20 min,75%B-100%B,20-30 min,100%B;柱温25℃;检测波长:白术内酯I(λ=276 nm)白术内酯II、白术内酯III、苍术酮(λ=220 nm),比较不同提取方法对白术有效成分的提取效果,同时考察不同有机溶剂、溶剂量、超声时间和超声次数等因素对白术超声提取的影响,最后得到白术供试样品的最佳制备方法。结果:选择超声离心提取方法,10 ml无水乙醇超声时间10 min,重复超声3次。结论:通过优化的白术多指标含量测定方法,可同时测定白术内酯I白术内酯II、白术内酯III、苍术酮四个指标成分,方法简单、高效、准确、稳定。
英文摘要:
      Objective: To establish a simple, efficient and accurate method for the determination of multi-indicator components in Atractylodes macrocephala Rhizoma through methods optimization. Methods: HPLC-DAD was used to determine the four indicator components of atractylenolide I, atractylenolide II, atractylenolide III and atractylon. Chromatographic conditions: The mobile phase was 0.1% phosphoric acid (A) and acetonitrile (B); Column used ZORBAX Eclipse XDB-C18 Analytical 4.6×250 mm 5-Micron; The gradient elution procedure was 0-8 min, 60% B, 8-16 min, 60% B-75% B, 16-20 min, 75 %B-100%B, 20-30 min, 100% B and column temperature was 25 ℃; Detection wavelength were atractylenolide I (λ = 276 nm) atractylenolide II, atractylenolide III, atractylon (λ = 220 nm). After comparing different extraction methods on active ingredients of Atractylodes macrocephala Rhizoma, at the same time, examine factors such as organic solvents, ultrasonic time, ultrasonic frequency and solvent amount were investigated. Finally, the best preparation method of Atractylodes macrocephala Rhizoma was obtained. Results: The method of ultrasonic centrifugation extraction was selected, 10ml absolute ethanol, ultrasound 10 min for 3 times. Conclusion: Through the optimized method of multi-index content determination of Atractylodes macrocephala Rhizoma, four indicators of atractylenolide I, atractylenolide II, atractylenolide III and atractyl alcohol can be simultaneously determined. The method is simple, efficient, accurate and stable.
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