ABSTRACT
Objectives To provide scientific basis for the quality control of different species of Baishouwu by establishing the HPLC fingerprint of domestic of Baishouwu and determining the main active components of acetophenones. Methods HPLC-DAD method was used to determine the HPLC fingerprints of domestic of Baishouwu. Then, the content of 4 kinds of acetophenones in Baishouwu was determined. The column was Diamonsil C18（250mm×4.6mm, 5μm）with the mobile phase of methanol and 0.1% phosphoric acid at a flow rate of 1.0 ml/min. The detection wavelength of p-Hydroxyl acetophenone, baishouwu benzophenone, 2',4'-Dihydroxy acetophenone was set at 260 nm and 2',5'-Dihydroxy acetophenone at 280 nm respectively. Results The similarity and cluster analysis in HPLC fingerprint showed that the constituents were significantly different among C. bungei, C. auriculatum and C. wilfordii. The content of total acetophenones in C. wilfordii was significantly higher than that in other localities of C. auriculatum and C. bungei. Conclusions Acetophenone could be used as the evaluation index to evaluate the quality of Baishouwu in different origins. The content of total acetophenone in C. wilfordii is the highest, which could be used as the best quality resource of Baishouwu.
ABSTRACT
HPLC specific chromatograms of Poria were established, and the concentrations of 10 triterpenoids(16α-hydroxydehydrotrametenolic acid, poricoic acid B, dehydrotumulosic acid, poricoic acid A, polyporenic acid C, poricoic acid AM, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, dehydropachymic acid, pachymic acid, and dehydrotrametenolic acid) were simultaneously determined. Chromatographic analysis was conducted on a Welch Ultimate XB C_(18) column(4.6 mm × 250 mm,5 μm). Acetonitrile solution(contain 3% tetrahydrofuran)(A) and 0.1% formic acid aqueous solution(B) were used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min~(-1). The column temperature was 30 ℃ and the injection volume was 20 μL. The experimental data were analyzed by the SPSS 22.0 and GraphPad Prism 7.0. The established triterpenoids fingerprints were specific, and the 10 components were well separated and showed good linearity(r≥0.999 6) within the concentration ranges tested. The mean recoveries were between 98.53%-103.8%(RSD 1.7%-2.7%). The method was specific and repeatable, and could be used for identification and quality evaluation of Poria. The results showed that the contents of 10 triterpenoids were positively correlated with each other. The contents of 10 triterpenoids of samples collected from producing areas were higher than that collected from markets. The total contents of 10 triterpenoids of samples collected from Hubei and Yunnan province were slightly higher than that from Anhui province, but the contents of samples from Anhui province were varied in smaller ranges.
Subject(s)
China , Chromatography, High Pressure Liquid , Materia Medica , Poria , ChemistryABSTRACT
To establish a method for simultaneous determination of the contents of sesamoside, menthyl chloride, chlorogenic acid, caffeic acid, 8-O-acetyl-phloridzin methyl ester, forsythiaside B, luteolin, and ergosterol, the LIPLC analysis was performed on a Kinetex XB-C₁₈ (4.6 mm×50 mm,2.6 μm)column with acetonitrile (A)-0.1% phosphoric acid solution (B) as the mobile phase. The flow rate is 1.0 mL min⁻¹. The detection wavelength was 238, 320 and 350 nm and column temperature was 30 ℃. The results showed that the eight components could be completely separated with good linear relationships (r≥0.999 8) in the linear range. The average recoveries were 96.61%-100.4%. The method was simple with strong specificity and high precision. It can be used for the identification and quality evaluation of the Lamiophlomis rotate.The results also showed that there was a correlation between the various components, and the habitat was the main factor affecting the content of the eight components. However, the degradation gradient had no obvious effect on the contents, while the content of sesamoside was significantly decreased after one year of storage.
ABSTRACT
Objective To establish a RP-HPLC method for the determination of 3-amide-indole derivative and its related substances. Methods Diamonsil C18(250 mmí4. 6 mm,5 μm) column was adopted. The mobile phase consisted of a mixture of methanol-acetonitrile-water(431245) at the flow rate of 1. 0 mL·min-1 . The wavelength for ultraviolet detection was 224 nm. The injection volume was 20 μL and the column temperature was room temperature. Results 3-amide-indole derivative and related substances could be well separated. The linearity of the 3-amide-indole derivative curve was well correlated (r=0. 999 7) within the range of 0. 04-0. 16 mg·mL-1. The RSD was 0. 52%with good repeatability. The detection limit was 2. 65 ng. Conclusion The method is accurate,reliable,sensitive and specific,which could be used for the determination of 3-amide-indolederivative and related substances.