ABSTRACT
Objective:Based on the previous studies, to investigate the dissolution behavior of Fuzi Lizhongwan by simultaneously determining the dissolution of benzoylmesaconine, benzoylaconine and benzoylhypaconine in Aconiti Lateralis Radix Praeparata. Method:The simultaneous determination of benzoylmesaconine, benzoylaconine and benzoylhypaconine in Fuzi Lizhongwan was established by HPLC-QQQ-MS. The dissolution amounts of three compositions in 15 batches of Fuzi Lizhongwan from 5 manufacturers at different time points, the cumulative dissolution was calculated and the dissolution curve was drawn. The f2 similarity factor method was adopted to evaluate similarity of dissolution curves of index components in different batches of samples from the same manufacturer, and to evaluate similarity of dissolution curves of samples from different manufacturers based on the same index component. The dissolution model of Fuzi Lizhongwan was concluded by fitting with the dissolution data. Result:When hydrochloric acid solution with pH of 1.2 was used as the dissolution medium, the three alkaloids had the best dissolution effect. The dissolution behavior of three monoester alkaloids in Fuzi Lizhongwan was basically synchronous and the dissolution lasted for 24 h. Three batches of samples from the same manufacturer (manufacturer 1, 3, 4 and 5) appeared to be similar on dissolution behavior, indicating that the dissolution behavior of the majority of samples from different manufacturers was similar. The dissolution behavior of batch 1 sample was different from batch 2 and 3 samples in manufacturer 2, suggesting that the quality of different batches of samples in manufacturer 2 might be different. The fitting results of dissolution data of index components in samples from different manufacturers were consistent, and the Weibull model was the best. Conclusion:Index components in fifteen batches of samples from 5 manufacturers are continuously dissolved within 24 h, indicating that the samples have the characteristics of slow dissolution. The dissolution curves of samples from the same manufacturer are similar to each other, indicating that the quality of different batches of products from most manufacturers is stable. The dissolution behavior of benzoylmesaconine, benzoylaconine and benzoylhypaconine in samples form different manufacturers has some differences, which may be caused by the source of medicinal materials and preparation technology parameters.
ABSTRACT
Objective: To research the process of extraction and purification of water-soluble alkaloids of Aconiti Lateralis Radix Praeparata (ALRP). Methods: Orthogonal design L9(34) and single factor experiments were employed to optimize the extraction conditions using UPLC-MS/MS. The total extraction yield of 14 alkaloids (karacoline, songorine, fuziline, neoline, talatisamine, mesaconine, aconine, hypaconine, benzoylmeaconine, benzoylaconine, benzoylhypaconine, mesaconitine, aconitine, and hypaconitine) was used as an index. The absorption-desorption characteristics of five macroporous resins were evaluated to optimize purification conditions using contents of eight water-soluble alkaloids (aconine, mesaconine, hypaconine, fuziline, neoline, talatisamine, songorine, and karacoline) as indexes. Results: The optimized extraction and purification conditions were as follows: steamed tablets were decocted thrice with 10-fold pH 3.5 acidic water for 2 h each time (maintaining pH 3.5). The alkalinity of water decoction was adjusted to pH 10.0 with 20% NaOH and then heated for 2 h. The supernatant was adjusted to pH 11.0 by 20% NaOH and then was subjected to macroporous resin HPD300 whose relative adsorption amount was 2.5 g dried medicinal herb/mL resin, and then the resin was eluted with 6 BV of water and 4 BV of 80% ethanol respectively. The 80% ethanol fraction was evaporated under vacuum to give the water-soluble alkaloids extract. The extract yield was 1.69%. The total contents of mesaconine, aconine, hypaconine, fuziline, neoline, talatisamine, karacoline and songorine were above 15%. Conclusion: The optimized extraction and purification process is stable and feasible, and this present study provides the reference for the research and application of water-soluble alkaloids in ALRP.
ABSTRACT
Objective To establish an HPLC method for the simultaneous determination of the 6 aconitum alkaloids in compoundTengwu Ointment.Methods Chromatographic column was Aglient XDB-C18 column (4.6 mm × 250 mm, 5μm), with the mobile phase A of acetonitrile- tetrahydrofuran (25∶8), phase B was 0.1 mol/L ammonium acetate solution (0.5 mL acetic acid added to the 1000 mL) with gradient elution;the flow rate was 1 mL/min;the detection wavelength was set at 235 nm;the column temperature was 25℃.Results Aconitine was in the good linear range of 0.072-0.648μg (r=0.999 5), with the average recovery of 99.29%, RSD=1.25%. Mesaconitine was in the good linear range of 0.062-0.648μg (r=0.999 5), with the average recovery of 99.12%, RSD=0.85%. Hypaconitine was in the good linear range of 0.064-0.384μg (r=0.999 8), with the average recovery of 99.57%, RSD=1.07%. Benzoylaconine was in the good linear range of 0.056-0.672μg (r=0.999 2), with the average recovery of 98.11%, RSD=0.61%. Benzoylmesaconine was in the good linear range of 0.055-0.993μg (r=0.999 9), with the average recovery of 99.27%, RSD=1.10%. Benzoylhypaconine was in the good linear range of 0.078-0.702μg (r=0.999 8), with the average recovery of 99.08%, RSD=1.38%.Conclusion This method is simple, sensitive, repeatable and accurate, which can be used for determination of aconitum alkaloids in compoundTengwu Ointment.
ABSTRACT
Objective: To investigate the effect of Aconiti Kusnezoffii Radix (AKR) combined with Trichosanthis Fructus (TF) in 13 different ratios on contents of benzoylmesaconitine, benzoylaconine, benzoylhypaconine, mesaconitine, aconitine, and hypaconitine. Methods: The powdered AKR-TF material, mixture, was alkalized by 10 times 75% ethanol and distilled water for 1 h, respectively, and extracted regurgitantly twice (each time for 1 h). The extracts were combined and centrifuged, and the supernatant was taken. The Welch Xtimate-C18 column (250 mm × 4.6 mm, 5 μm) was eluted with a mobile phase consisted of aceto-nitrile and 40 mmol/L ammonium acetate (pH value 10.0, adjusted with aqueous ammonia) and gradient elution at a flow rate of 1 mL/min. The eluent was monitored by a UV detector at 235 nm. Results: After AKR combined with TF, the content of monoester-alkaloids did not change significantly. Liquid pH value gradually reduced and total quality of diester-alkaloids increased with the ratios of TF increasing. Conclusion: From the view of chemical composition, the toxicity is increasing when AKR combined with TF.