| 王丽敏,周燕红,杨莹,等.白术多指标成分含量测定方法优化[J].浙江中医药大学学报,2020,44(7):657-667. |
| 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 |
| DOI：10.16466/j.issn1005-5509.2020.07.012 |
| 中文关键词: 白术 HPLC-DAD 白术内酯Ⅰ 白术内酯Ⅱ 白术内酯Ⅲ 苍术酮 多指标含量测定 方法优化 |
| 英文关键词: Atractylodes macrocephala Rhizoma HPLC-DAD atractylenolide Ⅰ atractylenolide Ⅱ atractylenolide Ⅲ atractylone multi-index content determination method optimization |
| 基金项目:浙江省公益技术研究计划项目(LGC20H280002)；国家重点研发计划项目—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) |
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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方法。[方法]采用高效液相色谱-二极管阵列检测器(high-performance liquid chromatography-diode array detection，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4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。采用ZORBAX Eclipse XDB-C18 Analytical 4.6mm×250mm 5-Micron色谱柱，柱温25℃。梯度洗脱程序:0～8min，60%B；8～16min，60%～75%B；16～20min，75%～100%B；20～30min，100%B。检测波长:白术内酯Ⅰ(λ=276nm)，白术内酯Ⅱ、白术内酯Ⅲ、苍术酮(λ=220nm)。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]经HPLC方法学考察、供试品溶液制备方法考察，最终选择以10mL无水乙醇为溶剂，超声离心提取，每次10min，重复3次，作为最佳样品制备方法。白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ、苍术酮分别在0.0015～0.1915mg·mL-1(r2=0.9999)、0.0085～0.1350mg·mL-1(r2=0.9999)、0.0015～0.3565mg·mL-1(r2=0.9998)、0.0145～0.9005mg·mL-1(r2=0.9999)范围内线性关系良好，平均加样回收率分别为98.45%、101.03%、100.11%、101.18%，相对标准偏差(relative standard deviation，RSD)分别为2.26%、3.29%、3.69%、2.14%。[结论]通过优化的HPLC-DAD白术多指标成分含量测定方法，可同时测定白术中白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ、苍术酮4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] High-performance liquid chromatography-diode array detection(HPLC-DAD) was used to determine the four indicator components of atractylenolide Ⅰ， atractylenolide Ⅱ， atractylenolide Ⅲ and atractylone in Atractylodes macrocephala Rhizoma. Chromatographic conditions: The mobile phase was 0.1% phosphoric acid(A) and acetonitrile(B); velocity of flow was 1.0mL/min； injection volume was 10μL； column used was ZORBAX Eclipse XDB-C18 Analytical 4.6mm×250mm 5-Micron， column temperature was 25℃. The gradient elution procedure was 0～8min， 60%B; 8～16min， 60%～75%B; 16～20min， 75%～100%B; 20～30min， 100%B. Detection wavelength was atractylenolide Ⅰ(λ=276nm)， atractylenolideⅡ， atractylenolide Ⅲ， atractylone(λ=220nm). After comparing different extraction methods on active ingredients of Atractylodes macrocephala Rhizoma， at the same time， 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] Through investigating the HPLC methodology and the preparation method of the test solution， the method of ultrasonic centrifugation extraction was selected， 10mL absolute ethanol as solvent， ultrasound 10mins for 3 times was the best sample preparation method. Atractylenolide Ⅰ， atractylenolide Ⅱ， atractylenolide Ⅲ and atractylone presented better linear relationship in the ranges between 0.0015～0.1915mg·mL-1(r2=0.9999)， 0.0085～0.1350mg·mL-1(r2=0.9999)，0.0015～0.3565mg·mL-1(r2=0.9998)， 0.0145～0.9005mg·mL-1(r2=0.9999). The average recoveries were 98.45%，101.03%，100.11%， 101.18% respectively. Relative standard deviations(RSDs) were 2.26%， 3.29%， 3.69%， 2.14% respectively.[Conclusion] Through optimized HPLC-DAD constituent content determination method of Atractylodes macrocephala Rhizoma， four indicators of atractylenolide Ⅰ， atractylenolide Ⅱ， atractylenolide Ⅲ and atractylone can be simultaneously determined. The method is simple， efficient， accurate and stable. |
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