枳壳炮制前后指纹图谱及主要黄酮类成分含量的变化

Changes of HPLC Fingerprint and Main Flavonoids Content of Aurantii Fructus Before and After Processing

目的:建立枳壳及其不同炮制品的HPLC指纹图谱,并对其所含的4种黄酮类成分进行定量分析。方法:采用HPLC,Inertsil ODS-3 C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.1%磷酸水溶液梯度洗脱,检测波长283 nm,流速1.0 m L·min^-1,建立生枳壳、麸炒枳壳和制枳壳的HPLC指纹图谱,通过相似度评价、聚类分析对枳壳炮制前后指纹图谱进行分析,并对芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷进行含量测定。结果:建立了枳壳及其炮制品的指纹图谱,以柚皮苷为参照峰,生枳壳标定了8个共有峰,麸炒枳壳标定了15个共有峰,制枳壳标定了11个共有峰,与各自对照指纹图谱的相似度均>0.95。芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷在炮制前的质量分数分别为0.574 7%,5.986 3%,0.302 2%,3.574 7%;经炮制后,上述4种成分在麸炒枳壳中的质量分数分别为0.948 4%,5.103 4%,0.549 3%,3.533 7%,在制枳壳中的质量分数分别为0.605 3%,4.762 3%,0.404 7%,3.264 9%。结论:枳壳的HPLC指纹图谱在炮制前后发生了显著变化。4种黄酮类成分含量在炮制前后均发生了一定程度的变化,样品中芸香柚皮苷、橙皮苷含量排序为麸炒枳壳>制枳壳>生枳壳,样品中柚皮苷、新橙皮苷含量排序则为生枳壳>麸炒枳壳>制枳壳。

Objective: To establish HPLC fingerprints of Aurantii Fructus and its processed products,and to quantitatively analyze the contents of four flavonoids in these products.Method: HPLC was employed with Inertsil ODS-3 C18 column(4.6 mm × 250 mm,5 μm),the mobile phase of acetonitrile-0.1% phosphoric acid aqueous solution for gradient elution,the detection wavelength of 283 nm,and the flow rate of 1.0 m L·min^-1.HPLC fingerprints of raw products,stir-fried bran products and processing products of Aurantii Fructus were established.Similarity evaluation and cluster analysis were used to analyze the chromatographic data.At the same time, the contents of narirutin, naringin, hesperidin and neohesperidin were determined.Result: HPLC fingerprints of Aurantii Fructus and its processed products were established,taking naringin as the reference peak,8,15,11 common peaks were demarcated for raw products,stir-fried bran products,processing products,respectively,the similarities of fingerprints were > 0.95.Contents of the above four flavonoids in raw products were 0.574 7%,5.986 3%,0.302 2% and 3.574 7%,respectively.After processing,the contents of these four components in stir-fried bran products turned into 0.948 4%,5.103 4%,0.549 3% and 3.533 7%,their contents in processing products turned into 0.605 3%,4.762 3%,0.404 7% and 3.264 9%,respectively.Conclusion: The HPLC fingerprint of Aurantii Fructus changes significantly before and after processing.The contents of four flavonoids change to a certain extent before and after processing.The order of contents of narirutin and hesperidin in samples was stir-fried bran products > processing products > raw products,while the order of contents of naringin and neohesperidin was raw products > stir-fried bran products > processing products.