ABSTRACT
Objective:To establish the fingerprints of Microctis Folium by ultra high performance liquid chromatography (UPLC); To determine the contents of three flavonoids in the Microctis Folium; To evaluate the quality difference of Microctis Folium from different producing areas. Methods:The fingerprints were performed on Agilent ZORBAX SB C18 column (2.1 mm×150 mm,1.8 μm). The mobile phase was acetonitrile - 0.1 % acetic acid solution with gradient elution at a flow rate of 0.30 ml/min. The column temperature was 30 ℃ and the detection wavelength was 315 nm. The common fingerprint peaks were identified by UPLC-mass spectrometry, and the identification results were confirmed by comparison of reference materials. Waters Cortecs T3 C18 chromatographic column (2.1 mm × 100 mm,1.6 μm) was used for content determination. The mobile phase was methanol-0.1 % formic acid solution with gradient elution at a flow rate of 0.35 ml/min. The column temperature was 30 ℃ and the detection wavelength was 339 nm. The contents of vitexin, isovitexin and narcissoside in 15 batches of Microctis Folium from different habitats were determine. Results:There were 11 common peaks in the fingerprint of Microctis Folium. Identified by mass spectrometry and confirmed by reference substance,10 chemical components were identified, including caffeic acid, p-hydroxycinnamic acid, ferulic acid, vitexin, isovitexin, kaempferol-3-O-rutoside, astragaloside, narcissoside, isorhamnetin-3-O-glucoside and linden glycoside. The similarity between the fingerprints of 15 batches of Microctis Folium and the control fingerprint was greater than 0.95, indicating that the overall similarity of the fingerprints of Microctis Folium from different producing areas was high. The total contents of three active components were 3.23-5.64 mg/g in Yangjiang City, Guangdong, 3.60-5.78 mg/g in Zhanjiang City, Guangdong, 4.68-5.73 mg/g in Yulin City, Guangxi and 3.87-5.21 mg/g in Wuzhishan City, Hainan . There was no significant difference in the content of three active components in different producing areas. Conclusion:The fingerprints and the determination method established in the study are stable and feasible, which can be used for the quality evaluation of Microctis Folium.
ABSTRACT
ObjectiveTo study the correlation between the appearance color of the sample powder and the contents of five non-sugar components of wine-processed Polygonatum kingianum rhizoma during processing， and determine the feasibility of color quantitative value for judging the processing end point of the wine-processed products， and to screen steroidal saponins and flavonoids as markers for the control of the wine-processed products during processing. MethodThe changes of apparent color of the sample powder at different time points of the wine-processed products were measured by colorimeter， and the total color value （E*ab），the total color difference value （ΔE*ab） were calculated. The contents of protodioscin， pseudoprotodioscin， dioscin， diosgenin and narcissoside in the wine-processed products （No. S0-S10） after processing for 0， 5， 10， 14， 16， 18， 20， 22， 24， 26， 28 h were determined simultaneously by ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS）. Cluster analysis （HCA）， principal component analysis （PCA）， partial least squares discriminant analysis （PLS-DA） and Pearson correlation analysis were used to analyze the chromaticity value of the sample powder and the content of the five components. ResultDuring processing of wine-processed P. kingianum rhizoma， E*ab of the sample powder showed a decreasing trend and the apparent color changed from light yellow to lacquer black. The contents of the five components showed an obvious dynamic change trend with time， and showed different laws. HCA results showed that the processing process of the wine-processed products could be divided into three stages， namely， the early stage （samples S0-S1）， the middle stage （samples S2-S4） and the late stage （samples S5-S10）. PCA results showed that there were significant differences in color and contents of five components between the initial sample and the processing samples， and the difference between samples S8 and S9 was the smallest. PLS-DA results showed that the variable importance in the projection （VIP） values of b*， the contents of pseudoprotodioscin， narcissoside， diosgenin and protodioscin were >1. Pearson correlation analysis showed that the contents of protodioscin， diosgenin and narcissoside had a significant positive correlation with E*ab （P<0.01）， the content of diosgenin had a significant negative correlation with E*ab （P<0.01）， while the content of pseudoprotodioscin had no linear correlation with E*ab. ConclusionIn the process of wine-processed P. kingianum rhizoma， there is a certain linear correlation between color quantitative value and chemical composition， and the processing end point can be determined objectively. It can be considered that protodioscin can be used as a marker for the control of the wine-processed products.
ABSTRACT
Objective:To develop a UPLC method for determining four glycosides in microctis folium.Methods:The UPLC deter-mination was performed on an Agilent SB -C18 (3.0 mm ×50 mm, 1.8 μm) colume with 0.05% acetonitrile -phosphate solution as the mobile phase.The detection wavelength was set at 320 nm.The flow rate was 0.3 ml· min-1.The column temperature was 25℃.Results:Narcissoside, isovitexin, kaempferol-3-rutinoside and isorhamnetin-3-O-glucoside all showed good linearity with the re-covery of 98.89%,99.03%, 97.00%and 97.41%, and RSD of 0.41%, 0.84%,0.44%and 0.80%, respectively (n=9).Con-clusion:The method is convenient with good stability , repeatability and sample recovery rate , which provides basis for the quality eval-uation and control of microctis folium.
ABSTRACT
Objective: To study the chemical constituents of Gynostema pentaphyllum. Methods: The chemical constituents were isolated and purified by silica gel, polyamide, and Sephadex LH-20 chromatography. Their structures were elucidated by physicochemical properties and spectral analysis. Results: Seventeen compounds were isolated and identified as dodecanoic acid (1), β-sitosterol (2), 3, 3', 5-trihydroxy-4', 7-dimethoxyflavanone (3), 1-2-benzenediol (4), 3'-O-methyltaxifolin (5), quercetin (6), rhamnetin (7), α-spinasterol-3-O-β-D-glucopyranoside (8), 3, 4-dihydroxy benzoic acid (9), narcissoside (10), L-rhamnosemono-hydrate (11), malonic acid (12), β-ethoxy-rutinoside (13), rutin (14), ombuoside (15), ginsenoside Rb1 (16), and β-daucosterol (17). Conclusion: Compound 1, 3-5, 7, 9, 10, and 12 are obtained from G. pentaphyllum for the first time.