中国中药杂志

2017, v.42(03) 531-535

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白术中内酯类成分的TLC鉴别与UPLC含量测定
Study on TLC identification and UPLC determination method of atractylenolide in Atractylodes macrocephala

赵玉娇;徐文慧;沈小丽;田俊生;秦雪梅;
ZHAO Yu-jiao;XU Wen-hui;SHEN Xiao-li;TIAN Jun-sheng;QIN Xue-mei;Modern Research Center for Traditional Chinese Medicine,Shanxi University;Taiyuan Tianzhong Yiyao Technology Co.,Ltd.;Heji Hospital Affiliated to Changzhi Medical College;

摘要(Abstract):

建立白术的薄层鉴别与其中3种内酯类成分含量同时测定方法。使用硅胶GF_(254)薄层板对白术进行定性鉴别;利用UPLC-PDA梯度洗脱法同时测定白术内酯Ⅰ,Ⅱ,Ⅲ,选用Waters BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),流动相为乙腈-水,检测波长235 nm。薄层鉴别特征明显,专属性强;含量测定的方法学考察结果符合规定,白术内酯Ⅰ,Ⅱ,Ⅲ线性关系良好(r>0.999 9),平均回收率分别为93.48%(RSD 1.4%),94.97%(RSD 1.6%),92.71%(RSD 1.2%)。所建立的白术薄层鉴别方法专属性强、重复性好,3种内酯类成分同时测定方法操作简单、灵敏度高,两者结合可以更好的用于白术的质量评价。
This research is to establish TLC and UPLC methods for simultaneous determination of 3 atractylenolides in Atractylodes macrocephala. Silica gel GF_(254) plate was used for identification of A. macrocephala,and UPLC-PDA gradient elution method was used to simultaneously determine atractylenolide Ⅰ,Ⅱ and Ⅲ. The Waters BEH C_(18)column( 2. 1 mm × 100 mm,1. 7 μm) with acetonitrile-water as mobile phase and the wavelength of UV detector of 235 nm were performed. The quality control study showed that the characteristic for identification by TLC was distinct and highly specific. The method of content determination was in accordance with the regulations. The quantitative evaluation of atractylenolideⅠ,Ⅱ and Ⅲ was in good linear range( r > 0. 999 9),and the average recovery was 93. 48%( RSD 1. 4%),94. 97%( RSD 1. 6%),92. 71%( RSD 1. 2%),respectively. TLC identification was in good specificity and repeatability,and the UPLC-PDA method for the simultaneous determination of 3 atractylenolides was simple and reliable for the quality control of A. macrocephala.

关键词(KeyWords): 白术;白术内酯;薄层鉴别;超高效液相色谱;质量评价
Atractylodes macrocephala;atractylenolide;TLC;UPLC;quality control

Abstract:

Keywords:

基金项目(Foundation): 国家国际科技合作计划项目(2011DFA32630);; 山西省科技计划项目(201603D321077);; 山西省科技创新重点团队项目(201605D131045-18);; 山西省重点实验室项目(201605D111004)

作者(Author): 赵玉娇;徐文慧;沈小丽;田俊生;秦雪梅;
ZHAO Yu-jiao;XU Wen-hui;SHEN Xiao-li;TIAN Jun-sheng;QIN Xue-mei;Modern Research Center for Traditional Chinese Medicine,Shanxi University;Taiyuan Tianzhong Yiyao Technology Co.,Ltd.;Heji Hospital Affiliated to Changzhi Medical College;

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DOI: 10.19540/j.cnki.cjcmm.20161222.074

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