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Study Of The Marigold Flower Fingerprints And Their Chemical Composition

Posted on:2012-04-23Degree:MasterType:Thesis
Country:ChinaCandidate:R SuFull Text:PDF
GTID:2214330338969601Subject:Drug analysis
Abstract/Summary:PDF Full Text Request
The marigold is the plant of marigold genera of the compositae, flower, leaf and root of which can be all made into medicine. The distribution of this plant is fairly wide in China in addition to the related resources. There are many active components in marigold such as carotene, flavone, lutein, essential oil, thiophene, etc, possessing many pharmacological actions including antioxygen, anticancer anti-gnat. It is believed to have high value of application in some fields: medicine and food possessing, for instance. This study applied several techniques such as chemometrics method, database, LC-MS and GC-MS to conduct the fingerprint and qualitative analysis of flavone, lutein esters and essential oil in order to display the chemical characters of marigold, by which the chemical components of marigold flower can be established and the basic data for the related studies such as the quality evaluation and control of marigold can be provided. To establish fingerprint and make qualitative analysis of some commonchromatographic peaks for the alcohol extraction of marigold flower. The chromatogram fingerprint is constructed with UV separated by high performance liquid chromatography (HPLC). Chromatographic condition included a ZORBAX Eclipse XDB chromatographic column (250 mm×4.6 mm, 5μm), gradient elution with acetonitrile and 2‰phosphoric acid solution, flow rate 1 mL·min-1, column temperature 25℃and detection wavelength 254 nm. LC-MS is required for qualitative analysis of some common chromatographic peaks. LC-MS performs on electrospray ionization source with negative ionization pattern scanning, nebulizer pressure pressure 35.0 psi and drying gas temperature 350℃, flow rate 10 L·min-1, scanned area 50-1 000 m/z. The chromatogram fingerprint of the alcohol extraction of marigold is composed of eight common chromatographic peaks and it is of better precision, repeatability and stability. The chemical compositions corresponded with five common chromatographic peaks are patuletin, isoquercitin, isoquercitrin, quercetagetin and its glycosidation.To establish fingerprint and make qualitative analysis of chromatographic peaks of lutein esters of marigold flower. Chromatographic condition included a ZORBAX Eclipse XDB chromatographic column (250 mm×4.6 mm, 5μm) with mobile phase as acetonitrile-methanol(A) and acetic ether(B), flow rate 1 mL·min-1, column temperature 25℃and detection wavelength 450 nm. An atmospheric pressure chemical ionization source (APCI) was used with a positive ion scan mode. Nebulizer pressure 60 psi, vaporizing chamber 450℃, drying gas flow rate 9 L·min-1, scanned area 50-1 000m/z. The chromatogram fingerprint of lutein esters of marigold is composed of ten chromatographic peaks, by LC-MS qualitative analysis to select six common chromatographic peaks which are All-trans-lutein laurate-myristate,All-trans-lutein dimyristate or All-trans-lutein laurate-palmitate,All-trans-lutein myristate-palmitate,All-trans-lutein dipalmitate or All-trans-lutein myristate-stearate,All-trans-lutein palmitate-stearate and All-trans-lutein distearate respectively. The fingerprint accords with the requirement of methodological validation and can be applied to the quality control of marigold.Fingeprint of essential oil in marigold was established, additionally with the accomplishment of the qualitative analysis of the chemical components. This study applied simultaneous distillation and extraction to extract essential oil; by GC-MS, the complete fingeprint of essential oil was found and the qualitative analysis for the separate peak of fingeprint was conducted, with combining Heuristic evolving latent projections (HEPL) of chemometrics method for the discrimination and resolution of the overlapping peak of chromatography. By area normalization method for chromatographic peak the relative amount of the compounds were obtained; on the basis of the principal chemical components plus with the application of principal component analysis (PCA) and clustering analysis (CA), the samples from different sources were classified. There are respectively favorable correlations concerning the degree of precision, repeatability, and constancy in the finger print of essential oil in marigold. There are 100 chemical components which take up more than 85 % of the total chemical components, and each of whose relative content proportion exceeds 1‰(the matching degree is above 90 %). The main chemical components include caryophyllene, ethyl palmitate, piperitone, spathulenol, myristic acid, (+)-calamene, andα-terpineol. The 18 samples can be classified into 3 sorts based on main chemical components.Complying with the requirement of the fingeprint analysis, this study established the fingeprint from the major regions of marigold. By LC- MS and GC- MS, the qualitative analysis of chromatographic peak was accomplished. Through this operation, the chemical characters of marigold could be more comprehensively and effectively displayed.
Keywords/Search Tags:marigold, alcohol extraction, lutein, essential oil, fingerprint, GC-MS, HPLC, Heuristic evolving latent projections (HEPL)
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