To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant e...To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion （CER）. Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows： the plant material powder was extracted with 70% ethanol （v/m = 60） by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl） and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl）, and purified by a CER column eluting with H2O and 70% ethanol （pH 10, adjusted with 25% aqueous ammonia）, successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.展开更多
Nano-assisted inclusion separation of alkali metals from basic solutions was reported by inclu sion-facilitated emulsion liquid membrane process. The novelty of this study is application of nano-baskets of calixcrown ...Nano-assisted inclusion separation of alkali metals from basic solutions was reported by inclu sion-facilitated emulsion liquid membrane process. The novelty of this study is application of nano-baskets of calixcrown in the selective and efficient separation of alkali metals as both the carrier and the surfactant. For this aim, four derivatives of diacid calix[4]-1,3-crowns-4,5 were synthesized, and their inclusion-extraction parameters were optimized including the calixcrown scaffold （4.4%, by mass） as the carrier/demulsifier, the commercial kero sene as diluent in membrane, sulphonic acid （0.2 mol.L-1） and ammonium carbonate （0.4 mol.L-1） as the strip and the feed phases, the phase and the treat ratios of 0.8 and 0.3, mixing speed （300 r.min-1）, and initial solute concentration （100 mg.L-1）. The selectivity of membrane over more than ten interfering cations was examined and the re sults reveled that under the optimized operating condition, the degree of inclusion-extraction of alkali metals was as high as 98%-99%.展开更多
目的对黄芪六一汤中黄芪总皂苷、黄芪总黄酮、黄芪多糖及甘草酸、甘草总黄酮、甘草多糖分别进行提取、分离,并筛选具有防治糖尿病肾病作用的药效组分。方法单因素法筛选树脂型号、上样浓度和体积、洗脱溶剂及用量建立大孔吸附树脂法对...目的对黄芪六一汤中黄芪总皂苷、黄芪总黄酮、黄芪多糖及甘草酸、甘草总黄酮、甘草多糖分别进行提取、分离,并筛选具有防治糖尿病肾病作用的药效组分。方法单因素法筛选树脂型号、上样浓度和体积、洗脱溶剂及用量建立大孔吸附树脂法对黄芪总皂苷、总黄酮进行富集分离;运用碱液萃取法对甘草酸、甘草总黄酮进行分离,采用水提醇沉法对黄芪多糖、甘草多糖进行纯化。12周龄雄性db/m小鼠8只作为对照组,将12周龄雄性db/db小鼠随机分为模型组、黄芪六一汤和各组分的高、低剂量(临床等效剂量的4、1倍)组,小鼠一般情况及血生化指标以盐酸罗格列酮片(RSG)为阳性对照;尿白蛋白(U-Alb)水平以缬沙坦分散片(API)为阳性对照,每组8只。各组小鼠分别在ig给药12周前、后,称质量。禁食12 h,自由饮水,收集24 h尿液,马斯亮蓝法检测24 h U-Alb浓度;尾静脉采血测空腹血糖(FBG);摘取眼球取血,采用全自动生化分析仪检测血清血肌酐(Scr)、尿素氮(BUN)、三酰甘油(TG)、总胆固醇(TC)含量。对照组、模型组及黄芪六一汤高、低剂量组小鼠肾组织经固定、石蜡包埋切片,Masson染色后,光学显微镜下观察。结果制得的黄芪总黄酮、黄芪总皂苷、黄芪多糖、甘草酸、甘草总黄酮、甘草多糖质量分数分别为(70.58±2.16)%、(72.97±1.06)%、(67.12±2.60)%、(81.02±1.04)%、(53.56±1.63)%、(64.62±1.27)%。与模型组比较,给予黄芪六一汤治疗后的各组小鼠肾纤维化程度较轻;与给药前比较,模型组小鼠体质量显著减轻(P<0.05),甘草总黄酮高、低剂量和甘草多糖低剂量组体质量显著降低(P<0.05、0.01),其他给药组无显著差异;与模型组比较,黄芪六一汤、黄芪总皂苷、黄芪多糖、黄芪总黄酮、甘草酸FBG、24 h U-Alb显著降低(P<0.05、0.01),黄芪总皂苷、黄芪六一汤、黄芪总黄酮、甘草酸组Scr显著降低(P<0.05、0.01),黄芪六一汤、黄芪多糖、甘草酸、黄芪总黄酮组BUN显著降低(P<0.05、0.01),黄芪六一汤、黄芪总皂苷、甘草酸、黄芪多糖高剂量组TG显著降低(P<0.05、0.01),黄芪六一汤、黄芪总皂苷、黄芪总黄酮、黄芪多糖组TC显著降低(P<0.05、0.01)。结论各组分确定的制备工艺稳定、科学、可行;黄芪总皂苷、黄芪总黄酮、黄芪多糖、甘草酸可能是黄芪六一汤防治糖尿病肾病的药效物质基础。展开更多
基金Scientific Research Foundation for the Returned Overseas Chinese Scholars by Ministry of Education of China (Grant No.[2004]527).
文摘To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion （CER）. Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows： the plant material powder was extracted with 70% ethanol （v/m = 60） by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl） and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl）, and purified by a CER column eluting with H2O and 70% ethanol （pH 10, adjusted with 25% aqueous ammonia）, successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.
基金supported by Islamic Azad University (Shahreza Branch)Iran Nanotechnology Initiative Council
文摘Nano-assisted inclusion separation of alkali metals from basic solutions was reported by inclu sion-facilitated emulsion liquid membrane process. The novelty of this study is application of nano-baskets of calixcrown in the selective and efficient separation of alkali metals as both the carrier and the surfactant. For this aim, four derivatives of diacid calix[4]-1,3-crowns-4,5 were synthesized, and their inclusion-extraction parameters were optimized including the calixcrown scaffold （4.4%, by mass） as the carrier/demulsifier, the commercial kero sene as diluent in membrane, sulphonic acid （0.2 mol.L-1） and ammonium carbonate （0.4 mol.L-1） as the strip and the feed phases, the phase and the treat ratios of 0.8 and 0.3, mixing speed （300 r.min-1）, and initial solute concentration （100 mg.L-1）. The selectivity of membrane over more than ten interfering cations was examined and the re sults reveled that under the optimized operating condition, the degree of inclusion-extraction of alkali metals was as high as 98%-99%.
文摘目的对黄芪六一汤中黄芪总皂苷、黄芪总黄酮、黄芪多糖及甘草酸、甘草总黄酮、甘草多糖分别进行提取、分离,并筛选具有防治糖尿病肾病作用的药效组分。方法单因素法筛选树脂型号、上样浓度和体积、洗脱溶剂及用量建立大孔吸附树脂法对黄芪总皂苷、总黄酮进行富集分离;运用碱液萃取法对甘草酸、甘草总黄酮进行分离,采用水提醇沉法对黄芪多糖、甘草多糖进行纯化。12周龄雄性db/m小鼠8只作为对照组,将12周龄雄性db/db小鼠随机分为模型组、黄芪六一汤和各组分的高、低剂量(临床等效剂量的4、1倍)组,小鼠一般情况及血生化指标以盐酸罗格列酮片(RSG)为阳性对照;尿白蛋白(U-Alb)水平以缬沙坦分散片(API)为阳性对照,每组8只。各组小鼠分别在ig给药12周前、后,称质量。禁食12 h,自由饮水,收集24 h尿液,马斯亮蓝法检测24 h U-Alb浓度;尾静脉采血测空腹血糖(FBG);摘取眼球取血,采用全自动生化分析仪检测血清血肌酐(Scr)、尿素氮(BUN)、三酰甘油(TG)、总胆固醇(TC)含量。对照组、模型组及黄芪六一汤高、低剂量组小鼠肾组织经固定、石蜡包埋切片,Masson染色后,光学显微镜下观察。结果制得的黄芪总黄酮、黄芪总皂苷、黄芪多糖、甘草酸、甘草总黄酮、甘草多糖质量分数分别为(70.58±2.16)%、(72.97±1.06)%、(67.12±2.60)%、(81.02±1.04)%、(53.56±1.63)%、(64.62±1.27)%。与模型组比较,给予黄芪六一汤治疗后的各组小鼠肾纤维化程度较轻;与给药前比较,模型组小鼠体质量显著减轻(P<0.05),甘草总黄酮高、低剂量和甘草多糖低剂量组体质量显著降低(P<0.05、0.01),其他给药组无显著差异;与模型组比较,黄芪六一汤、黄芪总皂苷、黄芪多糖、黄芪总黄酮、甘草酸FBG、24 h U-Alb显著降低(P<0.05、0.01),黄芪总皂苷、黄芪六一汤、黄芪总黄酮、甘草酸组Scr显著降低(P<0.05、0.01),黄芪六一汤、黄芪多糖、甘草酸、黄芪总黄酮组BUN显著降低(P<0.05、0.01),黄芪六一汤、黄芪总皂苷、甘草酸、黄芪多糖高剂量组TG显著降低(P<0.05、0.01),黄芪六一汤、黄芪总皂苷、黄芪总黄酮、黄芪多糖组TC显著降低(P<0.05、0.01)。结论各组分确定的制备工艺稳定、科学、可行;黄芪总皂苷、黄芪总黄酮、黄芪多糖、甘草酸可能是黄芪六一汤防治糖尿病肾病的药效物质基础。
