Preparation optimization for two inclusion compounds of erinacine A and their stabilities / 中成药

AIM To optimize the preparation of two inclusion compounds of erinacine A and to evaluate their stabilities.METHODS With feed ratio,milling time and milling speed as influencing factors,inclusion rate and yield as evaluation indices,the preparation was optimized by orthogonal test.The obtained inclusion compounds were characterized by infrared spectrophotometry and TLC,whose stabilities at high temperature (60 ℃),strong light (3 000 1x) and high humidity [(90 ±5)％] were investigated.RESULTS The optimal β-cyclodextrin inclusion conditions were determined to be 5 ∶ 1 for feed ratio,60 min for milling time,and 300 r/min for milling speed,the inclusion rate and yield were 20.66％ and 88.21％,respectively.The optimal hydroxypropyl-β-cyclodextrin inclusion conditions were determined to be 25 ∶ 1 for feed ratio,90 min for milling time,and 400 r/min for milling speed,the inclusion rate and yield were 69.25％ and 96.31％,respectively.The inclusion of Hericium erinaceus 80％ ethanol extract was physical process without composition change.At high temperature and strong light,two inclusion compounds' appearance showed no obvious change with little loss of erinacine A,which was just the contrary at high humidity.The inclusion effect of hydroxypropyl-β-cyclodextrin inclusion compound was better than that of β-cyclodextrin inclusion compound.CONCLUSION Both β-cyclodextrin and hydroxypropyl-β-cyclodextrin inclusion compounds of erinacine A exhibit good heat stability and light stability,but deliquescence can easily happen to them.

Preparación y crracterización de compuestos de sociación entre el acetato, proopionato y butirato de rodio(ii) con ß-ciclodextrina / Preparation ad ccharacterizaton of compounds of association between rhodium((ii) carboxylates (acetate, propionate and butyrate) and ß-cyclodextrln / Preparaçãoe caraacterização de compostos de associação ente o acetato, prropionato e butirato de ródio(ii) com ß-ciclodextrina

En el presente trabajo se describe la preparación y caracterización del acetato, propionato y butirato de rodio(II), y sus respectivos compuestos de inclusión y/o asociación con ß-ciclodextrina (ßCD). Estos complejos fueron caracterizados por análisis elemental (CHN), espectroscopia de absorción en la región de infrarrojo (IR), análisis térmico (TG/DTG/ DSC), difracción de rayos X en polvo (DRX), espectroscopia de resonancia magnética nuclear de protón y de carbo-no-13 (RMN ¹H, 13C). Además, se realizaron experimentos para la determinación de tiempos de relajación longitudinal (T1 lH) en Cross Polarization Magic Angle Spinning (CP/MAS). Los resultados encontrados a través de estos métodos indican la formación de compuestos de asociación y/o inclusión parcial entre los carboxilatos de rodio(II) acetato, propio-nato y butirato con ß-ciclodextrina.

This article describes the preparation and characterization of rhodium (II) acetate, propionate and butyrate, and their inclusion and/or association compounds with ß-cyclodextrin (ßCD). The characterization of the compounds in this study was performed by elemental analysis (CHN), FTIR spectroscopy, thermal analysis (TG/DTG/DSC), XRD powder pattern diffraction, ¹Hand 13C nuclear magnetic resonance in solution 13C, and 31PCP/ MAS NMR in solid state. Besides, experiments for the determination oflongitudinal T1 relaxation times were also used. The results indicated the formation of inclusion or association compounds between rhodium (II) carboxylates (acetate, propionate or butyrate) and ß-cyclodextryn.

Neste artigo descreve-se a preparação e caracterização de acetato, propionato e butirato de ródio(II), seus respectivos compostos de inclusão ou associação com ß-ciclodextrina (ßCD). Estes compostos de estudo foram caraterizados por análise elementar (CHN), espectroscopia de absorção na região de infravermelho (IV), análise térmica (TG/DTG/DSC), difração de raios-X em pó (DRX), espectrome-tria de ressonância magnética nuclear de próton e de carbono-13. Além disso, se conduziram experimentos para a determinação de tempos de relaxação longitudinal (Tj ¹H) em solução e de espectros no estado sólido de 13C CP-MAS, "Cross Polarization Magic Angle Spinning". Os resultados encontrados através desses métodos indicaram a formação de compostos de associação ou inclusão parcial entre os carboxilatos de ródio(II) acetato, propionato e butirato com a ß-ciclodex-trina.

Studies on the Extraction of Volatile Oil in Leifengguan Granules and the Preparation of Their ?-CD Inclusion Compounds / 中药新药与临床药理

Objective To optimize the conditions for the extraction of volatile oil from Fructus Tsaoko and Radix Saposhnikoviae in Leifengguan granules,and for the preparation of their ?-CD inclusion compounds.Methods With the percentages of extracted volatile oil of Fructus tsaoko and Radix saposhnikoviae as the target marker,single-element experiments were conducted to determine the optimum conditions for extracting the volatile oil.The application rate of included volatile oil was used as the target marker to optimize the conditions for including the oils with ?-CD.Results The optimized extraction conditions were: with 8-fold water added,the sliced herbal medicine of Fructus tsaoko and Radix saposhnikoviae should be extracted for six hours without advanced soaking with water.The optimized inclusion conditions were: applying the saturated aqueous solution method,15-fold 85 % ethanol was used to dissolve the volatile oil,the proportion of the above solution and ?-CD being 1︰8;at 25 ℃,the volatile oil was included for 30 minutes with ultrasonic wave.Conclusion The established process can be used for the extraction and the inclusion of volatile oil from Fructus Tsaoko and Radix Saposhnikoviae in Leifengguan granules.