枳壳和枳实化学成分的HPLC-ESI-MS分析

Chemical constituents of Fructus Aurantii and Fructus Aurantii Immaturus by HPLC-ESI-MS

目的分析比较枳壳、枳实的化学成分.方法采用HPLC-ESI-MS法,Symmetry ShieldTMRP18色谱柱(150 mm×3.9 mm,5 μm)(Waters,Milford,MA,USA).流动相:A为0.6%醋酸水溶液,pH=2.5;B为甲醇.采用梯度洗脱:20%～40%B(0～48 min),40%B(48～54 min),40%～55%B(54～60 min),55%～95%B(60～75min),95%B(75～85 min),95%～20%B(85～90 min).体积流量:0.7 mL/min.温度为室温,检测波长为283 nm.Surveg质谱检测器.结果鉴定了柚皮苷、柚皮苷元、新橙皮苷、橙皮苷、辛弗林等成分,并测定了它们在枳壳、枳实中的含量.枳壳、枳实药材的主要化学成分种类相同,但含量不同.结论HPLC-ESI-MS法可用于枳壳和枳实的研究.

Objective To analyze the chemical components of Fructus Aurantii (FA) and Fructus Aurantii Immaturus (FAI).Methods HPLC-ESI-MS with Surveg mass spectrometer was used in the study.Chromatographic column: Symmetry Shield TM RP_ 18 (150 mm×3.9 mm, 5 μm) (Waters, Milford, MA, USA); mobile phase: (A) water (0.6% HAc, pH=2.5), (B) methanol. Gradient elutions: 20%- 40% B (0-48 min); 40% B (48-54 min); 40%-55% B (54-60 min); 55%-95% B (60-75 min); 95% B (75-85 min); 95%-20% B (85-90 min).Flow rate and wavelength were 0.7 mL/min and 283 nm at room temperature, respectively.Results Four kinds of flavonoids were identified as naringin, neohesperidin, naringenin, and hesperidin, synephrine was also identified in FA and FAI. Furthermore, the contents of them were determined individually.The results showed that the chemical constituents in FA and FAI were the same but the contents were different.Conclusion HPLC-ESI-MS method can be efficiently used to study FA and FAI.