| Objective Traditional Chinese Medicine Cinnamomi Cortex is the dry bark of Lauraceae plant Cinmamomum cassia Presl.Traditionally,it was believed that Cinnamomi Cortex posseses the founctions to make up the fire,to help positive,ignition turns over to the Yuan,to dissipate cold which has penetrated the body,to relieve the pain to warm meridian and used for treating the erectile dysfunction cold uterus,the waist knee crymodynia,the kidney deficiency,deficient yang with upper manifestation dizziness with red eye,crymodynia,with heart and abdomen,cold-induced vomiting and diarrhea,cold hernia and abdominal pain,menstrual pain and amenorrhea.Modem Chinese materia medica research on the chemical constituents and pharmacological activities of Cinnamomi Cortex showed that it has many activities,such as anti-tumor,anti-SARS bacteriostasis and antioxidation activites,lower blood,glucose,lower blood-lipid and anti-thrombotic,aldose reductase inhibition,etc.In order to further reveal the material basis of Cinnamomi Cortex.We separated systematically the chemical constituents Cinnamomi Cortex.Using gas chromatography,liquid chromatography and mass spectrometry technology to qualitative analysis and quantitative analysis is one of the most important research direction and content of the effective chemical constituents of traditional Chinese medicine(TCM)research.To further investigate the effectieve material base of Cinnamomi Cortex,especially the trace compounds which are usually difficult to separate.The ultra high pressure liquid chromatography/mass spectrometry technology was used for analysis of numerous active euonymus natural active ingredients of medicinal materials.We established a rapid and accurate UPLC-ESI-MS qualitative analysis method,which could be developed and utilized to more rational application of Cinnamomi Cortex.It provides a scientific basis for the quality control of medicinal materials.This thesis is about the chemical constituents of Cinnamomi Cortex including petroleum ether extraction and methanol extraction parts,thoroughly research of the ethyl acetate extraction part,hoping that there are more compounds can be isolated.Methods:1.chemical constituents of Cinnamomi Cortex petroleum ether extraction part To study on the chemical constituents of Cinnamomi Cortex petroleum ether extraction parts,we used hydrodistillation and analysed by gas chromatography coupled to mass spectrometry(GC-MS)with compound library screening(NIST11.L).2.Study on the chemical constituents of Cinnamomi Cortex ethyl extraction part Cinnamomi Cortex(10 kg)was shattered to coarse powder and soaked with 8 times amount of 95% methanol(four times,each time 7 days).Then it was filtered combined,and concentrated to dense paste.The dense paste was reconstituted with suitable amount of water,extracted with ethyl acetate,water saturated n-butanol and the organic phase was collected.Organic phase was concentrated with reduced pressure.To study the chemical constituents from ethyl acetate extraction,silica gel column chromatography with positive and reversed phase,glucan gel column chromatography(Sephadex LH-20)and the preparative liquid chromatography,TLC(thin layer chromatography)method were used to isolated and purified the compounds from Cinnamomi Cortex..The structure were elucidated by combination of nuclear magnetic resonance spectrum,mass spectra analysis,physical and chemical properties,together with compare to the literature.3.chemical constituents of Cinnamomi Cortex methanol extraction part To analyze and identify the chemical constituents from the methanol extraction part of Cinnamomi Cortex,a qualitative analytical method of Ultra liquid chromatography coupled with time-of-flight tandem mass spectrometry(UPLC-TOF-MS)was developed.The analysis was performed on an ACQUITY CSH C18 column(100 mm×2.1 mm,2.5 ?m).The mobile phase consisted of acetonitrile and 0.1% formic acid was used for gradient elution,the flow rate was 0.3m L/min.Time of flight-mass spectrometry was applied for the qualitative analysis under both positive and negative modes and ESI was used for ion source in mass spectrometry.Results:1.96 compounds were separated and 67 of them were identified from the petroleum ether extraction part of Cinnamomi Cortex,accounting for 97.202% of the total peak area.The major components quantitatively calculated by area normalization method were: Cinnamaldehyde(22.07%);Methylcyclohexane(6.83%);1,1-Dimethyl cyclo--pentane(5.93%);1,3-Dimethylcyclopentane(5.29%).2.32 compounds were isolated from ethyl acetate extraction parts of Cinnamomi Cortex,and 26 compounds were identified by using modern spectroscopy technology(UV,IR,HR-ESI-MS,1H-NMR,13C-NMR).The isolated compounds were identified as 1-phenylpropane-1,2,3-triol(1),(-)-(7S,8R)-dihydrodehydrodi conifery alcohol(2),Polystachyol(3),7,4'-di-O-methyl-(+)-catechin(4),1-Phenyl-1,3-propanediol(5),2,3-Dihydroxy-1-(4-hydroxy-3,5-dimethoxyphenyl)-1-propanone(6),styrene glycol(7),Syringaresinol(8),(-)-secoisolariciresinol(9),1-(4-hydroxy-3-methoxyphenyl)-2-(4-(3-hydroxy-1-propenyl)-2-methoxyphenoxy)-1,3-Propanediol(10),Mevalonolactone(11),Erythro-1-C-syringylglycerol(12),glycerin-1-benzoatel benzoate(13),1,10-Seco-4?-hydroxy-muurol-5-ene-1,10-diket-one(14),Syringic acid(15),zhebeiresinol(16),(-)-gynuraone(17),Cassiferaldehyde(18),2-Methoxy cinnamic acid(19),3?-(1?-Hydroxyethyl)-7-hydroxy-1-isobenzo-furanone(20),cinnamic acid(21),Syringaldehyde(22),coniferyl aldehyde(23),(-)-isolariciresinol(24),Ciwujiatone(25),Methyl homovanillate(26).Compounds 1?2?5?6?7?9?10?11?12?13?14?16?17?20?25?26 were isolated from Cinnamomi Cortex for the first time.Compounds 16?17 were obtained from this genus plants for the first time.3.UPLC-TOF-MS was usded for qualitative analysis of Cinnamomi Cortex methanol extraction parts.This technique took advantage of the efficient separation ability and highly sensitive detection ability of MS.A qualitative analysis method based on UPLC-TOF-MS was established.With the positive and negative ions mass spectrum information and elements analysis and comarison with related literatures and reference substance data,29 compounds from the methanol extraction part of Cinnamomi Cortex were identified.This provides a scientific basis for quality control of the Cinnamomi Cortex and was helpful to stabilize its clinical curative effect and to interpret its action of mechanism.Conclusion:This thesis was based on Cinnamomi Cortex,including the efficient separation of chemical composition and rapid detection,which providing a methodology for the study of Traditional Chinese Medicine(TCM)for modernization by explore feasible techniques and methods.Using all kinds of modern instruments to detected and identified the chemical constituents of Cinnamomi Cortex,provide the theological evidences to the authenticity identification... |
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