Comparison of eleven active components in Lonicerae Japonicae Flos,Lonicerae Japonicae Caulis and leaves of Lonicero japonica by UPLC / 中国中药杂志

This present study aims to establish a UPLC method for simultaneously determining eleven components such as new chlorogenic acid,chlorogenic acid,caffeic acid,cryptochlorogenic acid,artichoke,isochlorogenic acid A,isochlorogenic acid B,isochlorogenic acid C,rutin,hibisin and loganin in Lonicerae Japonicae Flos,Lonicerae Japonicae Caulis and leaves of Lonicera japonica and comparing the differences in the contents of phenolic acids,flavonoids and iridoid glycosides of Lonicerae Japonicae Flos,Lonicerae Japonicae Caulis and leaves of Lonicera japonica.The method was carried out on an ACQUITY UPLC BEH C18column(2.1 mm×100 mm,1.7 μm) by a gradient elution using acetonitrile and 0.1% phosphoric acid.The flow rate was 0.3 mL·min-1.The column temperature was maintained at 30 ℃.The sample room temperature was 8 ℃.The wavelength was set at 326 nm for new chlorogenic acid,chlorogenic acid,caffeic acid,cryptochlorogenic acid,artichoke,isochlorogenic acid A,isochlorogenic acid B and isochlorogenic acid C,352 nm for rutin and lignin,and 238 nm for loganin.The injection volume was 1 μL.The eleven components has good resolution and was separated to baseline.Each component had a wide linear range and a good linear relationship(r≥0.999 6),the average recovery rate(n=9) was 98.96%,100.7%,97.24%,97.06%,99.53%,96.78%,98.12%,95.20%,95.12%,100.2%,98.61%and with RSD was 2.5%,1.4%,1.9%,2.1%,1.7%,1.9%,1.6%,2.0%,1.4%,2.2%,2.0%,respectively.Based on the results of the content determination,the chemometric methods such as cluster analysis and principal component analysis were used to compare the Lonicerae Japonicae Flos,Lonicerae Japonicae Caulis and leaves of Lonicera japonica.The results showed that Lonicerae Japonicae Flos and leaves of Lonicera japonica were similar in the chemical constituents,but both showed chemical constituents difference compored to Lonicerae Japonicae Caulis.The established multi-component quantitative analysis method can provide a reference for the quality control of Lonicerae Japonicae Flos,Lonicerae Japonicae Caulis and leaves of Lonicera japonica.

Drying model, kinetics, and stability of four rattan Chinese medicinal materials / 中草药

Objective: To establish the common model of four kinds of rattan traditional Chinese medicinal materials (TCMM) (Paederiae Scandens Caulis, Lonicerae Japonicae Caulis, Polygoni Multiflori Caulis, and Ipomoea batatas Caulis) determinate the drying kinetic parameters, and study the stability of active ingredients in the drying process. Methods: The experimental data of four rattan TCMM were fitted to the nine thin layer models (Page, Wang and Singh, Two-term exponential, Newton, Logarithmic, Aghbashlo, Two-term, Midilli, Diffusion approach) at the temperature of 40, 50, 60, and 70 ℃. R2, χ2, and RMSE were used as the criterion of fit. Fick diffusion law was used to calculate the drying dynamical parameters. Based on the principle of chemical kinetics, the stability of active ingredients in the drying process was studied. Results: Aghbashlo model was the best one to describe drying process of four rattan TCMM. The effective moisture diffusion coefficients D and activation energy Ea of four rattan TCMM were between 1 × 10−10 and 1 × 10−9 m2/s and 40—50 kJ/mol respectively. The degradation reactions of ursolic acid, THSG, and polysaccharide conformed to the first-order kinetic equation. The content of chlorogenic acid increased with the drying temperature and drying time increased. Conclusion: The drying dynamical parameters values of TCMM with different parts have different ranges, their drying process should be described by a common model. The quality of TCMM was affected greatly by drying process.

Applicability Study on QAMS for Multi-component Content Determination of Lonicerae Japonicae Caulis / 中国中医药信息杂志

Objective To establish a QAMS method for content determination of six compositions (chlorogenic acid, caffeic acid, cryptochlorogenin acid, isochlorogenic acid A, isochlorogenic acid C and loganin) from Lonicerae Japonicae Caulis; To verify the feasibility and applicability of this method in quality control of Lonicerae Japonicae Caulis. Methods Chlorogenic acid was set as internal reference substance. The HPLC analysis was performed on a Waters Symmetry C18 column (4.6 mm × 250 mm, 5 μm) with a mobile phase consisted of acetonitrile and 0.4% phosphoric acid solution in gradient elution manner at a flow rate of 1 mL/min. The column temperature was maintained at 35 ℃, and the detection wavelength was set at 327 nm for chlorogenic acid, caffeic acid, cryptochlorogenin acid, isochlorogenic acid A, isochlorogenic acid C and 236 nm for loganin. Results The relative correction factors of caffeic acid, cryptochlorogenin acid, isochlorogenic acid A, isochlorogenic acid C and loganin were established; there was no obvious difference between calculated value of QAMS and measured value of external standard method. Conclusion The quality control mode of QAMS can be used for multi-index synchronization quality evaluation of the six compositions from Lonicerae Japonicae Caulis.

A new organic acid from Lonicerae Japonicae Caulis produced in Shandong / 中草药

Objective: To study the chemical constituents of Lonicerae Japonicae Caulis produced in Shandong Province. Methods: Compounds were isolated and purified by repeated column chromatographies including silica gel, MCI-gel resin, Sephadex LH-20, and so on. Their structures were elucidated by spectral data, including extensive 1D and 2D NMR techniques. Results: Four compounds were obtained and identified as 11,14,15-trihydroxy-12-octadecenoic acid methyl ester (1), ochnaflavone (2), β-daucosterol (3), and loganin (4). Conclusion: Compound 1 is a new organic acid named as loniceric acid ester, and compound 2 is isolated from Lonicerae Japonicae Caulis for the first time.

Optimization of processing parameters for extraction of chlorogenic acid in Fule Granula using Box-Behnken experimental design / 中国生化药物杂志

Objective To optimize the processing parameters for the extraction of chlorogenic acid in Fule Granula by Box-Behnken experimental design.Methods The content of chlorogenic acid in Fule Granula was determination.The separation was performed on a Agilent ZORBAX Eclipse XDB C18 column(4.6 mm ×250 mm, 5 μm), and column temperature 30 ℃.Aetonitrile-0.2% H3PO4 was used as the mobile phase.The detection wavelength was at 327 nm.A three-factor and three-level Box-Behnken experimental design was employed to investigate effects of extraction time, solid-liquid ratio and extraction times on composite score of extracting amount of chlorogenic acid.Results Optimum process conditions were as follows:12 times the amount of water extracted three times, each time 60 min; chlorogenic acid extraction rate of 3.379%.Conclusion This optimized extraction technology has good predictability by Box-Behnken experimental design, and overall desirability, it provides a reference for application of Fule Granula.