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目的:建立适用于枳实提取物的化学成分分析及多组分同时定量测定的准确、灵敏的分析方法, 并用于该提取物的质量研究。方法:采用高效液相色谱-二极管阵列-电喷雾-串联质谱法(HPLC-DAD-ESI-MS/MS)。色谱分离采用C18色谱柱, 以乙腈-2%甲酸为流动相进行梯度洗脱。定性分析采用负离子全扫描和多级扫描模式, 多组分同时定量测定采用DAD检测器于283nm检测。结果:从枳实提取物中鉴定了18个化合物, 包括12个黄酮, 5个香豆素和1个柠檬苦素, 并建立了同时定量测定其中12个主要化合物的定量分析方法。另外还研究了该12个化学成分在ESI-MS/MS中的裂解规律, 为该提取物化学成分分析提供依据。该提取物的全面深入研究尚未见报道。结论:方法学验证表明所建立的方法快速、准确, 可有效用于枳实提取物的化学成分与多组分同时定量测定。本研究工作将为枳实提取物及相关药物制剂的质量研究提供技术支持。
OBJECTIVE: To establish an accurate and sensitive analytical method suitable for the simultaneous determination of chemical constituents and multi-components in Fructus Aurantii Immaturus extract, and to study the quality of this extract. Methods: The HPLC-DAD-ESI-MS / MS was used to determine the content of p-toluenesulfonamide. The chromatographic separation was performed on a C18 column eluting with a gradient of acetonitrile-2% formic acid as the mobile phase. Qualitative analysis using negative ion full scan and multi-level scanning mode, simultaneous determination of multi-component using the DAD detector at 283nm detection. RESULTS: Eighteen compounds, including 12 flavones, 5 coumarins and 1 limonin, were identified from the citrus aurantium extract, and the quantitative analysis method for simultaneous determination of 12 major compounds was established. In addition, the cleavage regularities of these 12 chemical components in ESI-MS / MS were also studied, which provided the basis for the chemical composition analysis of this extract. The comprehensive study of the extract has not been reported yet. Conclusion: The methodological verification shows that the established method is rapid and accurate and can be used for the simultaneous quantitative determination of the chemical constituents and multi-components in the Fructus Aurantii Immaturus extract. This research will provide technical support for the quality research of the citrus aurantium extract and related pharmaceutical preparations.