基于GC-MS及HPLC-PDA对四花青皮活性成分的分析

Analysis of chemical constituents in Citri Reticulatae Pericarpium Viride‘Sihuaqingpi’by GC-MS and HPLC-PDA

目的:对四花青皮挥发性化学成分进行GC-MS分析,并结合HPLC-PDA对其6种主要活性成分进行定量分析。方法:采用水蒸气蒸馏法提取四花青皮中的挥发油,结合GC-MS分析其化学成分及相对含量,进一步建立HPLC方法同时测定四花青皮中6种活性成分辛弗林、橙皮苷、川陈皮素、3,5,6,7,8,3′,4′-七甲氧基黄酮、橘皮素、5-羟基-6,7,8,3′,4′-五甲氧基黄酮的含量。结果:采用GC-MS分析从四花青皮中分离鉴定出的38种挥发性化合物,包括25种萜烯类、2种酯类、4种醇类、2种醛类、2种酚类、3种其他化合物。其中主要成分为柠檬烯(55.45%)、γ-松油烯(16.18%)、2-(甲氨基)苯甲酸甲酯(5%)、α-蒎烯(2.84%)以及β-蒎烯(2.75%)等。HPLC-PDA定量结果显示,四花青皮中活性成分以黄酮类为主,其中以橙皮苷的含量最高,多甲氧基黄酮类中,橘皮素、3,5,6,7,8,3′,4′-七甲氧基黄酮、川陈皮素的含量较高,而5-羟基-6,7,8,3′,4′-五甲氧基黄酮含量较低。结论:建立了四花青皮的GC-MS和HPLC-PDA的分离鉴定方法,该法简便易行,可为四花青皮药材的深入质量评价及体内药效物质的阐明提供有效数据。

OBJECTIVE To conduct GC-MS analysis on the volatile chemical components of Sihuaqingpi,and to quantitatively analyze its six main active components in combination with HPLC-PDA.METHODS Above all the volatile oil of SHQP was extracted by steam distillation and further identified by GC-MS.The extraction rate of the volatile oil was 0.77%.Then the contents of hesperidin,synephrine,tangeretin,nobiletin,3,5,6,7,8,3',4'-heptamethoxyflavone(HMF),5-hydroxy-6,7,8,3',4'-pentamethoxyflavone(5-HPMF)in SHQP were determined by HPLC.RESULTS A total of 38 chemical constituents were identified from SHQP,including 25 terpenes,2 esters,4 alcohols,2 aldehydes,2 phenols and 3 other compounds.Its main components were limonene(55.45%),γ-terpinene(16.18%),benzoic acid,2-(methylamino)-,methylester(5%),α-pinene(2.84%),β-pinene(2.75%).The HPLC-PDA results showed that the active components in SHQP were mainly flavonoids,with the highest content of hesperidin.The contents of tangeretin,HMF and nobiletin in polymethoxylated flavonoids were higher,while the content of 5-HPMF was lower.CONCLUSION GC-MS and HPLC-PDA methods were established to separate and identify the chemical compounds in SHQP,which were simple and workable and could provide effective data for in-depth quality evaluation of SHQP and elucidation of the pharmacodynamics in vivo.