Two new sucrose cinnamates from Polygonum lapathifolium var. salicifolium / 中国中药杂志

Two new sucrose cinnamates(1 and 2) along with nine known compounds(3-11) were isolated from ethanol extract of Polygonum lapathifolium var. salicifolium by silica gel column chromatography, ODS column chromatography and semi-preparative HPLC. Their structures were elucidated by extensive spectroscopic methods including 1 D-and 2 D-NMR experiments, as well as HR-ESI-MS analysis. Eleven compounds(7 sucrose cinnamates, 3 phenylpropanoids and 1 lactone) were obtained and their structures were identified as(1,3-O-di-p-coumaroyl)-β-D-fructofuranosyl-(2→1)-α-D-glucopyranoside(1),(1,3-O-di-p-coumaroyl)-β-D-fructofuranosyl-(2→1)-(6-O-acetyl)-α-D-glucopyranoside(2),(3-O-feruloyl)-β-D-fructofuranosyl-(2→1)-(6-O-p-coumaroyl)-α-D-glucopyranoside(3), hydropiperoside(4), vanicoside C(5),(1,3-O-di-p-coumaroyl)-β-D-fructofuranosyl-(2→1)-(6-O-feruloyl)-α-D-glucopyranoside(6), vanicoside B(7),trans-p-hydroxycinnamic acid methyl ester(8), trans-p-hydroxycinnamic acid ethyl ester(9), methyl ferulate(10) and dimethoxydimethylphthalide(11), respectively. Compounds 1 and 2 were two new sucrose cinnamates, and compounds 1-11 were isolated from this plant for the first time. The antioxidant activities of the isolated compounds 1-9 were investigated by an oxygen radical absorbance capacity(ORAC) assay, and all nine compounds were found to show strong antioxidant activities. Among them, compound 6(10 μmol·L~(-1)) was the supreme one in antioxidant activities, with its ORAC value equivalent to(1.60±0.05) times of 50 μmol·L~(-1) Trolox.

Simultaneous Determination of the Contents of 5 Indicator Components in Yanyan Tablets by QAMS / 中国药房

OBJECTIVE： To establish QAMS method for content determination of paeoniflorin， rutin， oroxin B， baicalin and cinnamates in Yanyan tablets. METHODS： HPLC method was adopted. The determination was performed on Hypersil GOLD-C18 column （250 mm×4.6 mm，5 μm） with mobile phase consisted of methanol-0.35％ phosphoric acid solution （gradient elution） at flow rate of 1 mL/min. The detection wavelengths were set at 280 nm （rutin， oroxin B， baicalin， cinnamates） and 230 nm （paeoniflorin）. The column temperature was 30 ℃， and sample size was 10 μL. Using paeoniflorin as internal reference， relative correction factors （RCF） of rutin， oroxin B， baicalin and cinnamates were established. Effects of different chromatogram system， chromatogram column， mobile phase proportion， flow rate and column temperature on relative correction factors were investigated； the chromatographic peaks of the components were located according to the relative retention time. The content of paeoniflorin as internal reference was determined by external standard method， and the other four components were determined by QAMS， and then compared with the results of external standard method. RESULTS： The separation degree of each component to be measured was greater than 1.5. The linear range was 3.97-119.22 μg/mL for paeoniflorin，1.96-58.68 μg/mL for rutin，2.39-71.64 μg/mL for oroxin B， 1.92-57.51 μg/mL for baicalin， 0.54-16.24 μg/mL for cinnamates（r≥0.999 7）， respectively. RSDs of precision， reproducibility and stability tests were all lower than 2％. Average recoveries were 97.20％-98.07％（RSD＜3％，n＝6）. RCFs of rutin， oroxin B， baicalin and cinnamates were 0.554 6，1.815 6，2.489 3 and 5.423 2， using paeoniflorin as internal reference. RSDs of RCF and relative retention time were all lower than 5％ under different chromatogram conditions. Absolut relative error of four components （except for internal reference） in 10 batches of Yanyan tablets sampled by QAMS and external standard method were all less than 1％. The results of the two methods were identical. CONCLUSIONS： The established method is accurate， rapid， efficient and inexpensive， and it can be used for simultaneous determination of 5 indicator components in Yanyan tablet.