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South Tinglizi Quality Standards And Multi-ingredient Content Determination

Posted on:2011-05-25Degree:MasterType:Thesis
Country:ChinaCandidate:J R LiFull Text:PDF
GTID:2204360305979003Subject:Drug Analysis
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In this paper, five compounds were isolated from the Semen Descurainiae, which are quercetin-3-O-β-D-glucopyranosyl-7-O-β-D-gentiobioside, kaempferol-3-O-β-D-glucopyranos-yl-7-O-β-D-gentiobioside, isorhamnetin-3-O-β-D-glucopyranosyl-7-O-β-D-gentiobioside, iso-rhamnetin-3,7-di-O-β-D-glucopyranoside andβ-daucosterol. Four compounds of flavonoids andβ-daucosterol were identified by MS and NMR. The purity of four flavonoids compunds were bigger than 98%. they can be used for multi-determination.To establish a method which can determine the content of quercetin-3-O-β-D-glucopyranosyl-7-O-β-D-gendobioside in Semen Descurainiae and Semen Descurainiae Tostum. The chromatographic conditions are as follows, MP C18 column, acetonitrile-water(0.1%acetic acid) 11:89 as mobile phase,detection wavelength at 254 nm, the follow rate 1.0 mL·min-1,the temperature of column 25℃. The liner range is 0.15625-1.5625μg for the reference compound. The average recovery was 99.12%and RSD 1.28%. Through the result of 28 batches of the herb, the content of quercetin-3-O-β-D-glucopyranosyl-7-O-β-D-gentiobioside in Semen Descurainiae should not be less than 0.075%. The content in Semen Descurainiae Tostum should not be less than 0.08%.According to the appendix of Pharmacopoeia 2005 edition, carried out identification and inspection studies of Semen Descurainiae and Semen Descurainiae Tostum. Determine the shape and microscopic characteristics of them. In TLC polyamide thin-film method, quercetin-3-O-β-D-glucopyranosyl-7-O-β-D-gentiobioside as a reference substance to obtain a good separation. The provisions of the Semen Descurainiae ingredients:water content of no more than 9.0%, total ash content of the provisions of no more than 8.0%, acid insoluble ash content of the provisions of no more than 3.0%. Semen Descurainiae Tostum:water content defined as no more than 5.0%, total ash content of the provisions shall not exceed 8.0%, acid insoluble ash content defined as no more than 3.0%.The quality standards of Semen Descurainiae and Semen Descurainiae Tostum have been incomed in the first part of 2010 edition Chinese Pharmacopoeia (P313-314).Character identification and powder microscopic identification could make a distinction for Semen Descurainiae and Semen Descurainiae Tostum. The Stir-Frying does not make a difference for the content of quercetin-3-O-β-D-glucopyranosyl-7-O-β-D-gentiobioside as the indicator substance.Therefore,there were no distinction in TLC and the fererence substance content by HPLC for Semen Descurainiae and Semen Descurainiae Tostum.This paper has also established the simultaneous determination method of four compounds of flavonoids and sinapine thiocyanate in Semen Descurainiae.The conditions are as follows: column was Venusil MP C18 (250 mm×4.6 mm,5μm), a mobile phase of acetonitrile-water (0.08 mol/L KH2PO4) as mobile phase, gradient elution, detection wavelength 254 nm, flow rate was 1.0 mL·min-1; column temperature was 25℃. The determination results of 25 herbal was comprehensive analyzed. By the calculation, the average content of quercetin-3-O-β-D-glucopyr-anosyl-7-O-β-D-gentiobioside was 0.096%, kaempferol-3-O-β-D-glucopyranosyl-7-O-β-D-gent-iobioside was 0.0256%, isorhamnetin-3-O-β-D-glucopyranosyl-7-O-β-D-gentiobioside was 0.0673%, isorhamnetin-3,7-di-O-β-D-glucopyranoside was 0.0267% and the sinapine thiocyanate was 0.498%.
Keywords/Search Tags:Semen Descurainiae, Chemieal constituents, Semen Descurainiae Tostum, HPLC, Quality standard
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