焦白术饮片质量标准的研究

Research on Quality Standards of Deep-Fried Atractylodes Macrocephala

目的:建立焦白术饮片的质量标准。方法:采用性状、显微鉴别法对焦白术饮片性状、显微特征进行描述;按照《中华人民共和国药典》方法对水分、总灰分、浸出物进行测定;用薄层色谱(TLC)法定性鉴别;采用高效液相色谱(HPLC)法测定白术内酯Ⅰ、Ⅱ、Ⅲ的含量,以Amethyst C18-H色谱柱(4.6 mm×250 mm,5μm);以乙腈-水为流动相,梯度洗脱,流速1.0 mL·min-1;柱温30℃;检测波长220 nm和276 nm。结果:显微特征明显,专属性良好;薄层鉴别方法斑点清晰,分离度良好;水分的平均值为3.2%,总灰分的平均值4.3%;浸出物平均值为71.8%;白术内酯Ⅰ、Ⅱ、Ⅲ含量平均值依次120.1、136.8、162.5μg·g^-1;并且与相邻峰完全分离,线性关系良好,加样回收率(n=6)依次为99.9%、93.6%和91.2%,RSD依次为1.3%、2.1%和2.6%。结论:本方法简单、专属性强,可用于焦白术饮片的质量控制,提升质量标准。

Objective:To establish quality standards of deep-fried Atractylodes macrocephala.Methods:The characters and microscopic characteristics of the decoction pieces of deep-fried Atractylodes macrocephala were described by means of morphological and microscopic identification.The contents of water、total ash and extractum were analysed according to the methods of Chinese Pharmacopoeia(2015).Qualitative identification was by thin layer chromatography(TLC).The content of atractylenolideⅠ、atractylenolideⅡand atractylenolideⅢwere analysed by HPLC method.The determination was performed on a C18 column(4.6 mm×250 mm,5μm)with acetonitrile-water as the mobile phase.The flow rate was 1.0 mL·min-1;column temperature was 30℃.The detection wavelength was 220 nm and 276 nm.Results:The microscopic features are obvious and the specificity was good.TLC method has clear spots and good separation degree.The average contents of water was 3.2%,total ash was 4.3%,extractum was 71.8%;The content of atractylenolideⅠ、atractylenolideⅡand atractylenolideⅢwere 120.1,136.8,162.5μg·g^-1 respectively.Adjacent peaks were completely separated and has a good linear relationship,the sample recovery(n=6)were 99.9%,93.6%,91.2%respectively,RSD was 1.3%,2.1%,2.6%respectively.Conclusion:This established method is simple,feasibleand specific,and can be effectively suitable for the quality deep-fried Atractylodes macrocephala.,and improve the quality standards.