Separation And Analysis Of Volatile Oils And Alkaloids From Lindera A Ggregata (Sims) Kosterm.

Lindera aggregata(Sims)Kosterm.is a traditional Chinese medicine,known as Tiantai Wuyao,has a wide range of pharmacological activities,its active components are mainly volatile oils,alkaloids,furan sesquiterpenes and its lactones.Domestic and foreign related researches mainly focus on furan sesquiterpenes and its lactones,while the studies on volatile oils and alkaloids are relatively few.Some studies have shown that volatile oils have antibacterial,antitumor and regulation of gastrointestinal functions,alkaloids have anti-inflammatory,antioxidant and antitumor effects.However,the volatile oils and alkaloids in Wuyao are complex and low in content,and the traditional method of separation and analysis is inefficient.This paper adopts the modern separation and analysis methods such as GC-MS,LC-MS and high-speed countercurrent chromatography(HSCCC)to study the volatile oils and alkaloids of Tiantai Wuyao.The major results are shown as following:1.The effects of soaking time,solid-liquid ratio and extraction time on the extraction efficiency of volatile oils from Tiantai Wuyao were studied by using traditional distillation method.The optimum extraction conditions were as follows:soaking time 3 h,liquid ratio 12 mL/g,extraction time 3 h.The analysis method of the chemical compositions of volatile oils was established by GC-MS,and 39 chemical components of the volatile oil were determined by searching the standard spectral library and comparing with the relevant literatures.The results show that this method is fast and the volatile components with low content has good analysis effect,which is applicable to the analysis of volatile oil components in Tiantai Wuyao.2.Study on extraction of alkaloids in Tiantai Wuyao by ultrasonic assisted solvent extraction and acid water alkaline treatment.HPLC analysis method was established by optimizing the parameters such as mobile phase,flow rate and so on,then analyzed the components of alkaloid extracts by HPLC-MS.The accurate molecular weight of some alkaloids were analyzed by high performance liquid chromatography-high resolution mass spectra and obtained the molecular formulas.The ion fragments were obtained by HPLC-ESI-MS/MS,and referring to the related references,6 chemical compounds pallidine.norboldine?pronuciferine?norisoboldine?boldine and reticulline were deduced.And the fragmentation pathway of the isoquinoline alkaloids from Tianyai Wuyao was studied.The experimental results show that this method has high sensitivity and quick analysis,and is especially suitable for rapid screening and detection of trace alkaloids in Tiantai Wuyao.3.A HSCCC method with the suitable solvents system consisting of n-butanol-ethyl acetate-0.5%acetic acid(4:1:5,v/v)was investigated to separate alkaloids from Tiantai Wuyao.28.6 mg of norisoboldine and 7.2 mg of boldine were obtained from 400 mg of alkaloid extracts with the purities were 95.27%and 93.61%.The structures were identified by NMR spectrum.The result suggested that HSCCC can gain target compound with high purity,greater yield,and is a chromatographic separation method with higher separation efficiency,which indicates that HSCCC is suitable for separating alkaloids from Tiantai Wuyao.