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ObjectiveTo compare the four preparation methods of Rehmanniae Radix juice described in ancient literature and find the method that is most suitable for the preparation of Rehmanniae Radix juice used in Baihe Dihuangtang. MethodThe ancient medical books record four methods for preparing Rehmanniae Radix juice： crushing fresh Rehmanniae Radix for juice， steaming fresh Rehmanniae Radix for juice， boiling fresh Rehmanniae Radix for juice， and boiling dry Rehmanniae Radix for juice. Ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry （UPLC-Q-TOF-MS） was employed to detect the compounds in the four juice samples， followed by principal component analysis （PCA）. Result① Totally 27 compounds were identified in the juice samples， including 10 iridoid glycosides， 14 phenylethanoid glycosides， 2 phenolic acids， and 1 irisone. Among them， 15 common compounds were shared by the four juice samples， including 7 iridoid glycosides， 7 phenylethanoid glycosides， and 1 phenolic acid. ② Five common compounds in the four juice samples can be matched with the reference standards， which were catalpol， aucubin， rehmannioside D， ajugol， and purpureaside C. ③ Verbascoside and isoacteoside were not detected in the juice prepared by crushing fresh Rehmanniae Radix， while it was detected in the other three juice samples， which indicated that the two components were produced after heating rather than being the original components in fresh Rehmanniae Radix. ④ The comparison of the ion fragments demonstrated that verbascoside was produced from purpureaside C after the cleavage of the glycosidic bond and removal of a molecule of mannose. ⑤ Isoacteoside could be isomerized from verbascoside， and its relative content increased with the extension of heating time. However， the relative content of verbascoside and purpureaside C did not decrease significantly. Therefore， it was hypothesized that purpureaside C was produced from its upstream component. ConclusionThe juice prepared by crushing fresh Rehmanniae Radix has the chemical composition significantly different from the juice samples prepared with the other 3 methods， while the latter 3 juice samples had similar chemical composition. Although all the four methods can be used， it is more suitable to prepare Rehmanniae Radix juice by steaming fresh Rehmanniae Radix， boiling fresh Rehmanniae Radix， and boiling dry Rehmanniae Radix.
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Objective: The optimum extraction process parameters of Cistanche deserticola were selected to study the effects of different drying methods on five phenylethanoid glycosides. Methods: Single factor screening combined with Box-Behnken response surface method was used to optimize the extraction process. After optimal conditions were extracted, HPLC method was used to detect the content of echinacoside, cistanche A, verbascoside, isoacteoside, and 2’-acetylacteoside in different drying methods, and one-way ANOVA, cluster analysis, principal component analysis and close value analysis were used to analyze the content of five phenylethanoid glycosides to choose the best drying method. Results: Optimal extraction process was as following: methanol volume fraction was 55.14%, liquid to material ratio was 46.39, extraction time was 38.50 min. Cluster analysis, principal component analysis, and close value analysis showed that the quality of C. deserticola obtained by freeze-drying method was the best, followed by drying at 80 ℃ and the lowest at 40 ℃. Conclusion: Using this process to extract C. deserticola, the five phenylethanoid glycosides are completely and fully extracted. Although the freeze-drying method of C. deserticola has the highest active ingredient retention, from the production point of view, the 80 ℃ drying method can achieve a balance of cost and efficiency.
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Objective:To establish a HPLC fingerprint detection method of Plantaginis Semen, and analyze the samples from different producing areas in Jiangxi province by combining with chemical pattern recognition method, and the contents of five ingredients in Plantaginis Semen were determined. Method:A total of 34 batches of Plantaginis Semen medicinal materials were detected by HPLC. The similarity evaluation was carried out by the 2012 edition of similarity evaluation system of chromatographic fingerprint of traditional Chinese medicine. The chromatographic peak information was used as the data source, and three chemical pattern recognition methods were used to comprehensively analyze the quality of this medicinal herb. Quantitative analysis was performed on the 5 active components, including geniposidic acid, plantamajoside, acteoside, galuteolin and isoacteoside. Result:The similarities between Plantaginis Semen samples from different producing areas in Jiangxi province were >0.86. Orthogonal partial least squares-discriminant analysis (OPLS-DA) could distinguish samples from different producing areas, and be used to determine the chemical components, which had strong correlation with the quality of Plantaginis Semen. The contents of 5 active components in samples from different producing areas were different to some degree, especially in the content of plantamajoside. Conclusion:The established HPLC fingerprint of Plantaginis Semen has strong characteristics, combined with chemical pattern recognition method, it can effectively evaluate the quality of Plantaginis Semen and distinguish its producing areas.
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OBJECTIVE: To establish an HPLC method to simultaneously determine the contents of geniposidic acid, caffeic acid, acteoside and isoacteoside in Plantaginis Semen formula granules, in order to provide basis for studying its quality standards. METHODS: An HPLC method was developed. Kinetex C18 column (2.1 mm×100 mm, 2.6 μm)was used and eluted with mobile phase of 0.5% acetic acid-acetonitrile at the flow rate of 0.3 mL·min-1. The wavelength was set at 239 nm for geniposidic acid, 325 nm for caffeic acid, and 330 nm for acteoside and isoacteoside. The column temperature was maintained at 30℃. RESULTS: The good linear relationships between the concentration and peak area were in the range of 0.292 1-2.92 1 μg for geniposidic acid, 0.003 4-0.033 6 μg for caffeic acid, 0.047 6-0.476 μg for acteoside and 0.102 7-1.027 μg for isoacteoside (r≥0.999 8), respectively. The average recoveries were 99.32%, 98.62%, 98.23% and 98.51% with RSDs of 1.47%, 1.36%, 1.62% and 1.53%, respectively. CONCLUSION: The method is simple, feasible and reproducible and can be used for the quality control of Plantaginis Semen formula granules.
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Objective: The optimal simultaneous separation process of three phenylethanoid glycosides (acteoside, isoacteoside, and torenoside B) from Monochasmasavatieri were established using of macrophage resins and dynamic axial column (DAC). Methods: The adsorption/desorption experiments and dynamic separation experiments were performed on eight types of resins (AB-8, D 101, HPD 100, LSA-10, LX-11, LX-17, LX-38, and XDA-6) to find the optimal resin. Then the optimal separation parameters were investigated on the chosen resin. The total phenylethanoid glycosides obtained from the large-scale experiment were further seperated to get acteoside, isoacteoside, and torenoside B, respectively using of DAC system. Results: Among these candidate resins, LX-17 was chosen to further obtain the optimal parameters: The optimal feeding concentration of raw materials was 1.8 g/mL; The optimal adsorption time was 150 min; The optimal gradient elute conditions were ethanol/water (0/100, 4 BV; 15/85, 4 BV; 60/40, 5 BV; 90/10, 2 BV). The large-scale experiments were amplified to 10 folds on the basis of optimal parameters to obtain total phenylethanoid glycosides. Acteoside, isoacteoside, and torenoside B were simultaneously obtained from total phenylethanoidglycosides using DAC system. Conclusion: LX-17 and DAC system can be used for the purification of phenylethanoid glycosides, which will have a goodfuture for the application in industry.
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Objective: To study the chemical constituents from the whole plant of Goldfussia pentstemonoides. Methods: The compounds were separated and purified by chromatographic methods. The structures were identified by spectroscopic analyses. Results: Ten compounds were isolated from the n-butanol fraction of 95% ethanol extract in the whole plants of G. pentstemonoides and identified as salidroside (1), 1-(α-L-rhamnosyl-(1→6)-O-β-D-glucopyranosyloxy)-3,4,5-trimethoxybenzene (2), isoacteoside (3), isonuomioside A (4), benzyl-O-β-D-glucopyranoside (5), lcariside F2 (6), (-)-lyoniresinol 3α-O-β-D-glucopyranoside (7), (+)-isolariciresinol-9-O-β-D-glucopyranoside (8), decaffeoylverbascoside (9), and dehydrodiconiferyl alcohol 4-O-β-D-glucopyranoside (10). Conclusion: All compounds are isolated from G. pentstemonoides for the first time.
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Objective: An UHPLC-MS/MS method was developed for the simultaneous determination of acteoside, isoacteoside, and forsythoside B in plasma of rats and the pharmacokinetic parameters for three phenolic glycosides were calculated as well. Methods: Samples of plasma of rats were obtained at different time after rats were administrated with Callicarpa nudiflora extract (5 g/kg). After the addition of acidification (hydrochloric acid, 0.25 mol/L) and deproteinization by acetonitrile, plasma samples were separated on a Phenomenex® Kinetex C18 column (50 mm × 2.1 mm, 1.7 μm) with gradient elution using acetonitrile-0.005% formic acid as mobile phase. Mass spectrometric detection was carried out by multiple reaction monitoring (MRM) using electrospray ionization in negative ion mode. Results: A good linearity of acteoside, isoacteoside, and forsythoside B was shown in the ranges of 7.77 - 3 880.00 ng/mL (r2 = 0.995 5), 5.04 - 2 520.00 ng/mL (r2 = 0.994 9), and 1.78 - 890.00 ng/mL (r2 = 0.995 1), respectively. The mean extraction recoveries of analytes were in the range of 75.2% - 89.9%, and the intra- and inter-day RSD values were less than 8.8%. The tmax of acteoside, isoacteoside, and forsythoside B was about 30 min, AUC0~t were (93 881.65 ± 18 326.65), (29 204.97 ± 8 499.88), and (15 027.05 ± 3763.82) ng∙min/mL, Cmax were (2 179.00 ± 355.60), (737.57 ± 210.31), and (227.30 ± 48.38) ng/mL, t1/2z were (235.41 ± 117.90), (151.56 ± 49.23), and (161.68 ± 63.92) min, respectively. Conclusion: The method is proved to be simple, rapid, and specific, and to be suitable for the simultaneous determination of acteoside, isoacteoside, and forsythoside B in plasma of rats and the pharmacokinetic study.
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This study was aimed to establish an HPLC method for simultaneous determination of the content of echinacoside, acteoside and isoacteoside in Total Cistanchis glycosides Capsules. Waters C18 column (4.6 mm ×150 mm, 5 μm) was used with the mobile phase of methanol-0.1% formic acid at a flow rate of 1.0 mL·min-1. The detection wavelength was set at 330 nm. The column temperature was maintained at 30℃ . The results showed that the linear ranges of echinacoside, acteoside and isoacteoside were in the range of 27.792-277.92 μg·mL-1 (r = 0.9996,n = 6), 2.4184-24.184 μg·mL-1 (r = 0.9996, n = 6), 5.106-51.06 μg·mL-1 (r = 0.9998, n = 6). The average recoveries of three components were in accordance with the determination requirement. It was concluded that the method was simple and accurate, which can be used in the content determination of echinacoside, acteoside and isoacteoside in Total Cistanchis glycosides Capsules.