白术挥发油的HPLC定量质控和特征图谱研究

目的: 建立白术挥发油的HPLC定量质控和特征图谱分析方法,并分析比较4个产地挥发油中特征成分及其相对含量的异同点。 方法: 采用Hypersil ODS2(4.6 mm×250 mm,5 μm)色谱柱,流动相为乙腈(A)-水(B),梯度洗脱(0~30 min,40%B→10%B;30~40 min,10%B→10%B);流速1.0 mL·min^-1 ;定量质控检测波长:0~9 min时200 nm(白术内酯Ⅲ、β-桉叶醇),9.1~20 min时220 nm(白术内酯Ⅰ),20.1~45 min时200 nm(苍术酮、β-榄香烯);特征图谱检测波长205 nm;柱温30 ℃。 结果: 挥发油的HPLC定量质控和特征图谱分析方法学考察结果良好。浙江、安徽、湖南和河北等产地挥发油特征图谱与共有模式之间相似度≥0.998。4个产地挥发油特征图谱及共有模式之间特征峰的相对保留时间的RSD≤1%,相对峰面积RSD的范围为21%~79%。4个产地挥发油特征图谱及共有模式中的特征峰峰面积占总峰面积的97.10%~98.33%。浙江、安徽、湖南产地挥发油特征图谱及共有模式中的特征峰的相对保留时间RSD≤0.86%,相对峰面积的RSD≤2%;与河北的进行比较,相对峰面积RSD的范围为5.6%~68%。 结论: 建立的HPLC挥发油定量质控及特征图谱分析方法简单、稳定、可靠。4个产地挥发油特征图谱整体相似度较高,特征成分种类相近,但其相对含量有差异。浙江、安徽、湖南产地挥发油特征图谱中的特征成分的种类及其相对含量相近;河北产地挥发油特征图谱中的特征成分的相对含量与其他3个产地的相比存在一定差异。

Objective: To establish quantitative quality control and specific chromatograms analysis methods of Rhizoma Atractylodis Macrocephalae volatile oil by HPLC.Using the methods,the differences of feature chemical components and their relatively contents in the volatile oil from four different sources were compared. Methods: The methods were carried out by Hypersil ODS2(4.6 mm×250 mm,5 μm) column,using acetonitrile(A)-water(B) as mobile phase with gradient elution(0-30 min,40%B→10%B;30-40 min,10%B→10%B),at a flow rate of 1.0 mL·min^-1.The quantitative quality control detection wavelength was set at 200 nm(0-9 min) for atractylenolid Ⅲ and β-eudesmol,220 nm(9.1-20 min) for atractylenolid Ⅰ and 200 nm(20.1-45 min) for atractylon and β-elemene.The specific chromatograms detection wavelength was set at 205 nm.The column temperature was 30 ℃. Results: The HPLC methods of quantitative quality control and specific chromatograms for the volatile oil were established.The methodological results were good.The similitude degree of four different sources volatile oil specific chromatograms exceeded 0.998.As compared with the specific components peaks relative retention time and their relative peak area in the feature chromatograms gathered in four different sources volatile oil and mutual mode dates with each other,the RSDs range of the relative retention time were less than 1%,and the range of the relative peak areas RSDs were in 21%-79%.The sum of the specific peaks area in feature chromatograms and mutual mode of four different sources volatile oil accounted for 97.10%-98.33% of total peaks area.Compared with the specific components peaks relative retention time and their relative area of the feature chromatograms collected in Zhejiang,Anhui and Hunan sources volatile oil and mutual mode with each other,RSDs of the relative retention time and the relative peaks area were less than 0.86% and 2%,respectively.As adding dates of Hebei source volatile oil to compare,the range of the relative peak area RSDs were in 5.6%-68%. Conclusion: The established methods of quantitative quality control and specific chromatography for the volatile oil by HPLC were simple,accurate and reliable.The total similarity degree of the feature chromatograms gained in four different sources volatile oil were higher and the varieties of their feature components were very closely same,but the relative content of these components had some difference.The varieties and their relative content of specific components in the feature chromatograms collected in Zhejiangs,Anhuis and Hunans sources volatile oil were closely same,but the dates compared with these obtained from the Hebei sources volatile oil,the varieties of specific components were very similar,but their relative content had bigger difference.