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Studies On Chemical Components And Method Of Quality Assessment Of Xiangjiapi

Posted on:2008-12-05Degree:MasterType:Thesis
Country:ChinaCandidate:L TongFull Text:PDF
GTID:2144360215964451Subject:Drug Analysis
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Corex Periplocae is the dried root bark of Asclepiadaceae and Periplocca sepium Bge.. It has been recorded in the edition 2005 of Pharmacopoeia of the PRC for treating congestive heart failure and rheumatic arthritis. 15 Xiangjiapi samples were collected from different habitats, which were used for the studies on the chemical components and the method of quality assessment.The dried root bark of Xiangjiapi was extracted with 70% ethanol. By solvent extraction, various chromatographic techniques of isolation (Si gel CC, PTLC, Sephadex LH-20, Semi-preparative Chromatography) and recrystallization, 6 compounds were isolated and purified from CHCl3 extract. By means of spectroscopic analysis and physiochemical properties, 5 of them were identified as: lupeol,β-sitosterol, isovanillin, periplocoside M and daucosterol.The chemical compositions of essential oil from Xiangjiapi have been studied by GC-MS method. 17 constituents of essential oil were got and 13 of them were identifed. The total content of the identified compounds was 13.1%. The chemical compositions of fatty oil from Xiangjiapi have been studied by GC-MS and known substance reference methods. 22 fatty acid compounds were got and 20 of them were identifed. The total content of the fatty acids was 78.76% and the unsaured fatty acids was 41.72%. The content of palmitic acid was the highest (32.14%) and linoleic acid was the next (24.53%).A capillary gas chromatographic (CGC) method equipped with flame ionization detection was developed for the simultaneous analysis of palmitic acid, oleic acid and linoleic acid in Xiangjiapi. Compounds were separated on an Agilent DB-17 capillary column (30m×0.25mm i.d, 0.25μm). The polar column was 150℃programmed to 190℃at 2℃·min-1, 190℃for 10 min. Split radio, 10:1; detector temperature, 250℃. The orthogonal design was adopted to optimize the derivation reaction conditions of fatty oil. The optimal derivatization conditions of fatty oil were described as follows: sample was dissolved in 5 ml of a 0.5% w/v solution of sodium hydroxide in methanol in a 25 ml flask with a ground-glass stopper and boiled under a reflux condenser for 45 min. 2.0 ml boron trifluoride-ether solution was added through the condenser and boiled for 5 min. The calibration curves were linear in the range of 0.025~0.250 mg·ml-1(r=0.9998)for palmitic acid, 0.019~0.190 mg·mL-1(r=0.9994)for oleic acid and 0.087~1.045 mg·ml-1(r=0.9992) for linoleic acid, respectively. The average recovery of palmitic acid was 99.2%(RSD=3.3%); oleic acid, 99.4%(RSD=2.6%); linoleic acid, 100.2%(RSD=2.9%). The assay method was simple, rapid, reliable and reproducible and provided a quantitative basis for the quality assessment of Xiangjiapi.A RP-HPLC method was developed for simultaneous determination of isovanillin, periplocin and 4-methoxy salicylaldehyde in Xiangjiapi. A Kromasil C18 column was used with the mobile phase being acetonitrile-water-phosphoric acid system, gradient elution and the detection wavelength was set at 230 nm. The orthogonal design was adopted to optimize the extraction of isovanillin, periplocin and 4-methoxy salicylaldehyde. The optimal extracting condition was methanol consumed ten times the amount of material, and three times for 20 min each time. The linear ranges for isovanillin, periplocin and 4-methoxy salicylaldehyde were 1.6~13.7μg·mL-1(r=0.9996), 4.9~49.2μg·mL-1(r=0.9994) and 5.0~99.4μg·mL-1(r=0.9996), respectively. The average recoveries were 101.7%(RSD=1.3%), 99.5%(RSD=2.5%)and 99.9%(RSD=2.0%), respectively. The assay method was simple, rapid, reliable and reproducible and provided a quantitative basis for the quality assessment of Xiangjiapi.In this study, 6 compounds were isolated and purified from CHCl3 extract of Xiangjiapi; the chemical components of essential oil and fatty oil from Xiangjiapi were studied, and the simultaneous analysis of 3 kinds of fatty acids was developed; a new methodology was developed for simultaneous determination of isovanillin, periplocin and 4-methoxy salicylaldehyde in Xiangjiapi. The quality assessment of Xiangjiapi should be helpful explore as a new quality assessment method for traditional Chinese medicines.
Keywords/Search Tags:Xiangjiapi, GC-MS, Fatty acid, Isovanillin, Periplocin
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