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OBJECTIVE： To optimize the extraction technology of osthole from the pine needles of Cedrus deodara. METHODS： HPLC method was adopted to determine the content of osthole. Based on single factor test， ethanol volume fraction， extraction time and material-solvent ratio were selected as influential factors， and the content of osthole was selected as response value. Box-Behnken design-response surface methodology was used to optimize the extraction technology of osthole in pine needles of C. deodara. Validation test was conducted. RESULTS： The optimal extraction technology was as follows as ethanol volume fraction of 88％， material-solvent ratio of 1 ∶ 20 （g/mL）， extracting for 2 times， lasting for 57 min each time. Under this technology， average content of osthole was 0.675 7 mg/g （RSD＝1.78％， n＝3）， and the relative error of which to predicted value 0.680 9 mg/g was 0.59％. CONCLUSIONS： The optimal extraction technology is simple and feasible，and it can be used for the extraction of osthole from the pine needles of C. deodara.
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Objective: To research the simultaneous purification process of shikimic acid and total flavonoids from pine needles of Cedrus deodara (Roxb.) G. Don. Methods: Taking the purity of shikimic acid and total flavonoids as the evaluation indicator, the purification effect of six macroporous resins were evaluated. Orthogonal design L9(34) and single factor experiments were employed to optimize the purification conditions by comprehensive scoring. The purification capacity of the best resin was investigated by the sample mass concentration, the volume flow of the sample, the ratio of the resin to the drug, the amount of water for washing, the concentration of ethanol, and the elution of ethanol. Results: XAD 7HP macrophous resin offered better purification effect of shikimic acid and total flavonoids from pine needles of C. deodara than other macrophous resins. The optimum purification condition was confirmed as follows: The concentration of shikimic acid in the sample was 11.59 mg/mL, and total flavonoids concentration was 6.9 mg/mL; The flow rate was 8 BV/h, and the sample volume was 2.0 mL/g; The shikimic acid was eluted with loading capacity and 4 BV of water; The total flavonoids was eluted with 4 BV of 70% ethanol successively. The purity of shikimic acid can be increased from 19.25% to 28.98%, and the purity of total flavonoids can be increased from 11.92% to 54.45%. Conclusion: The optimized purification process is stable, feasible and suitable for pilot enrichment of shikimic acid and total flavonoids from pine needles of C. deodara.
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OBJECTIVE:To optimize the extraction technology of total lignans from pine needles of Cedrus deodara. METH-ODS:Using ethanol volume fraction,ratio of liquid to solid and extraction time as response factor,the content of total lignans as response value,the response surface methodology test was conducted based on Box-Behnken design to optimize the extraction tech-nology of total lignans from pine needles of C. deodara. RESULTS:The optimal extraction technology was as follows as ethanol volume fraction of 78%,ratio of liquid to solid 25∶1,extraction time 1.75 h. The content of total lignans from pine needles of C. deodara was 99.2 mg/g,which was close to predicted value 100.49 mg/g,with relative deviation of 0.65%. CONCLUSIONS:Op-timized extraction technology of pine needles of C. deodara by response surface methodology is feasible and stable,and has good predictability.
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Objective: To investigate the chemical constituents in the n-butanol extract of pine needles of Cedrus deodara. Methods: Chemical constituents were separated and purified by silica gel and Sephadex LH-20 chromatography column. The structures were elucidated on the basis of physicochemical properties and spectral data (1H-NMR, 13C-NMR, and DEPT). Results: The compounds were identified as 1-(4'-hydroxy-3'-methoxyphenyl)-2-[4″-(3-hydroxypropyl)-2″-methoxyphenoxy]-1, 3-propanediol (1), (7S, 8R)-9, 9'-dihydroxy-3, 3'-dimethoxy-7, 8-dihydro-benzofuran-1'-propanol base neolignan-4-O-β-D-glucoside (2), (7R, 8R)-3', 9, 9'- trihydroxy-3-methoxy-7, 8-dihydro-benzofuran-1'-propanol base neolignans-9-O-α-L-rhamnoside (3), (6R, 9R)-6-hydroxy-3-oxo-α- ionol-9-O-β-D-glucopyranoside (4), (6R, 9R)-3-oxo-α-ionol-9-O-β-D-glucopyranoside (5), shikimic acid butyl ester (6), quinic acid butyl ester (7), (6S, 9R)-6-hydroxy-3-oxo-α-ionol-9-O-β-D-glucopyranoside (8), 5-p-trans-coumaroylguinic acid (9), and (E)-1-O-p- coumaroyl-α-D-glucopyranoside (10). Conclusion: Compounds 1-7 are isolated from C. Trew for the first time.
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Objective To study the chemical constituents of flavonoids in pine needles of Cedrus deodara.Methods Flavonoids were isolated and purified from ethyl acetate extract of pine needles by chromatography on silica gel and Sephadex LH-20.Their structures were identified on the basis of spectroscopic analysis and chemical evidence.Results Five flavonoids were isolated and purified.Their structures were identified as cedrusone A(1),myricetin(2),2R,3R-dihydromyricetin(3),quercctin(4),and 2R,3R-dihydroquercetin(5).Conclusion Compound 1 is a new compound.Compounds 2-5 are isolated from pine needles of this genus for the first time.
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Objective: To study the chemical constituents of flavonoids in the pine needles of Cedrus deodara. Methods: Flavonoids were isolated and purified from ethyl acetate extract of the pine needles by chromatography on silica gel and Sephadex LH-20. Their structures were identified on the basis of spectroscopic analysis and chemical evidence. Results: Five flavonoids were isolated and identified as 3′,5′-dimethoxymyricetin-3-O-(6″-O-acetyl)- α-D-glucopyranoside (1), myricetin (2), 2R,3R-dihydromyricetin (3), quercetin (4), and 2R,3R-dihydroquercetin (5). Conclusion: Compound 1 is a new compound named as cedrusone A. Compounds 2-5 are isolated from the pine needles in the plants of Cedrus Trew for the first time.