补骨脂素和异补骨脂素的分离纯化研究

应用高速逆流色谱技术分离和纯化补骨脂中香豆素类成分补骨脂素和异补骨脂素．以补骨脂干燥成熟果实为原料,经乙醇回流制备补骨脂粗提物,经高速逆流色谱分离,所得样品由高效液相色谱检测纯度,并由对照品确定成分．采用正己烷．乙酸乙酯-甲醇-水（7：3：5：5）作为两相溶剂体系,从补骨脂粗提物中分离得到补骨脂素和异补骨脂素,二者纯度分别达到99．4％,99．1％．该法可以成功用于补骨脂粗提物中补骨脂素和异补骨脂素的分离,并且具有制备量大和分离效率高的优点．     

补骨脂化学成分的分离与鉴定

从中药补骨脂(Psoraleacorylifolia)种子中通过溶剂提取、硅胶柱层析、SephadexLH 20柱层析和制备薄层层析等方法分得四个化合物。波谱分析(核磁共振氢谱、碳谱和质谱)确定它们的结构分别为补骨脂二氢黄酮甲醚(1,bavachinin)、补骨脂二氢黄酮(2,bavachin)、新补骨脂异黄酮(3,neobavaisoflavone)和补骨脂宁(4, cory lin)。     

Glycosidase inhibitory phenolic compounds from the seed of Psoralea corylifolia

The seeds of Psoralea corylifolia were extracted into five different polar solvents: chloroform, 50% ethanol in water, ethanol, methanol and water. All extracts were evaluated for glycosidase inhibitory activity. The chloroform extract (CE) showed the lowest IC₅₀ values against α-glucosidase (82.9 μg/ml) and α-mannosidase (132 μg/ml). Chromatography of CE yielded nine phenolic compounds which were identified as isovabachalcone (1), 4′-O-methylbavachalcone (2), isobavachromene (3), corylifolin (4), bavachinin (5), psoralidin (6), neobavaisoflavone (7), corylifol A (8), and bakuchiol (9). All isolated compounds, apart from compound 5, possessed α-glucosidase inhibitory activities. Among them, compounds 6–8 exhibited potent inhibition with IC₅₀s of 13.7, 27.7 and 11.3 μM, respectively. Furthermore, compounds 2 and 6 showed α-mannosidase inhibitory activity. Mechanistic analysis of their inhibition modes against α-glucosidase showed that compounds (6 and 7) were noncompetitive, whereas compound 8 was mixed. Furthermore, the most active glycosidase inhibitors (2, 6–8) were proven to be present in the native seed in high quantities by an HPLC chromatogram.     

超声-UPLC法测定补骨脂中补骨脂素和异补骨脂素

补骨脂是我国用于生产各种保健品的传统原料之一,其主要活性成分为补骨脂素和异补骨脂素。本实验改进中国药典补骨脂项下补骨脂素和异补骨脂素含量测定方法。采用C18ODS色谱柱(1.8μm,4.6 mm×50 mm),流动相乙腈-水(35∶65),流速0.5 mL/min,检测波长246 nm,测定药典法和超声法制备补骨脂供试品溶液中补骨脂素和异补骨脂素含量。5 min内补骨脂素、异补骨脂素分离良好。在相应浓度范围内2种化合物的线性关系良好,r>0.999 7;精密度RSD≤2%;平均加样回收率为>99%。超声法与索氏提取法相比无显著性差异(P>0.05)。该方法操作简便,节省时间和溶剂,为补骨脂中补骨脂素、异补骨脂素的分析提供了一种简便快速的新手段。     

补骨脂多糖的分离纯化、结构鉴定及其对RAW264.7巨噬细胞活力的影响

对补骨脂多糖（Psoralea corylifolia polysaccharides,PPs）进行分离纯化,并对多糖的一般理化性质、单糖组成、摩尔质量、红外光谱、核磁共振（nuclear magnetic resonance,NMR）谱（1H-NMR和13C-NMR）、微观结构及其对RAW264.7活力的影响进行研究。利用热水提取乙醇沉淀,除蛋白,经DEAE-52纤维素色谱柱（0.05 mol/L NaCl溶液洗脱）和Sephadex G-100柱色谱分离纯化得到2 种多糖（PPs-1-1和PPs-2-1）,均为白色絮状粉末,能溶于水,不溶于乙醇、正丁醇、丙酮、氯仿、石油醚等有机溶剂;考马斯亮蓝染色、斐林试剂反应、三氯化铁反应、碘-碘化钾反应均为阴性,总糖质量分数分别为（94.35±0.23）%和（95.27±0.42）%。PPs-1-1和PPs-2-1均由鼠李糖、阿拉伯糖、木糖、甘露糖、葡萄糖和半乳糖以不同物质的量比组成,平均摩尔质量分别为3.98×106 g/mol和4.47×106 g/mol;PPs-1-1具有表面光滑且致密的三维层流结构,具有α-和β-构型的呋喃糖苷;PPs-2-1具有表面疏松多孔的层状结构,具有β-构型的吡喃糖苷;PPs-1-1和PPs-2-1质量浓度分别低于0.16 μg/mL和0.01 μg/mL时,可明显激活RAW264.7巨噬细胞的活力。     

高效液相色谱法同时测定化妆品中香豆素等15种化合物

建立了同时测定化妆品中香豆素等15种化合物(双香豆素、4-羟基香豆素、香豆素、7-甲氧基香豆素、6-甲基香豆素、8-羟基补骨脂素、补骨脂素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、新补骨脂异黄酮、补骨脂二氢黄酮、三甲沙林、欧前胡内酯和异欧前胡内酯)的高效液相色谱分析方法。样品经甲醇超声提取,以10 000 r/min离心5 min,取上清液过滤后测定。采用Phenomenex Luna C18(2)(250 mm×4.6 mm,5μm)色谱柱分离,以乙腈-0.1%乙酸溶液为流动相梯度洗脱,流速1.0 m L/min,柱温30℃。采用二极管阵列检测器多波长(210,250和280 nm)检测,标准曲线法定量。结果表明,香豆素等15种化合物的线性范围为0.1~10.0 mg/L,相关系数均大于0.999,检出限(LOD)为0.1~0.7 mg/kg。在3种加标水平下的平均加标回收率为90.5%~106.4%,相对标准偏差为0.7%~3.4%(n=6)。该方法准确、简便,适用于化妆品中香豆素等15种化合物的测定。     

补骨脂对猪油抗氧化作用的研究

用OSI法测定了补骨脂原药材及补骨脂提取物对猪油的抗氧化作用。结果表明 ,补骨脂及补骨脂提取物有很强的抗猪油自动氧化的能力。石油醚提取物与氯仿提取物的抗氧化作用相当 ,且两者的抗氧化作用均强于 0 0 2 %的BHT。     

补骨脂抗癌成分的分离与鉴定

从中药补骨脂 (Psoraleacorylifolia)种子中通过溶剂提取、硅胶柱层析、SephadexLH 2 0柱层析和制备薄层层析等方法分得 4个化合物。波谱分析 (核磁共振氢谱、碳谱和质谱 )确定它们的结构分别为补骨脂素 ( 1,psoralen)、异补骨脂素 ( 2 ,isopsoralen)、补骨脂定 ( 3 ,psoralidin)和异补骨脂查尔酮 ( 4 ,isobavachalcone)。文献报道化合物 1～ 3有不同程度的抗癌作用     

补骨脂抗氧化性能及其有效成分的研究

用乙醚,乙酸乙酯、甲醇三种溶剂对补骨脂进行了提取,抗氧化性能测试表明乙醚提物效能最好。经过一系列分离纯化步骤,从中得到了一种抗氧化性能很强的单体化合物,其抗氧化性能明显强于ＢＨＡ。理化 性质和波谱分析证明该化合物为补骨脂里定。     

Antioxidant activities of selected oriental herb extracts

Antioxidant activities of methanol extracts of 180 Oriental herbs were studied by determining the peroxide values of linoleic acid during storage at 50°C. Among the herb extracts tested, 44 species showed strong antioxidant activities on the oxidation of linoleic acid. The antioxidative effects of these 44 selected herb extracts were studied further in a methyl linoleate system during storage for 35 d. Among the 44 species tested, 11 species had particularly high antioxidative effects. The effects of type of extraction solvent (methanol, petroleum ether and ethyl acetate) on the antioxidant activities of the 11 species were studied. Antioxidant activities of most herb extracts were greatly dependent on the extraction solvent used; however, some of the extracts showed strong antioxidant activities regardless of the solvents used for the extraction. Among the 11 herbs selected, based on the antioxidant activity of their methanol extracts, two (i.e.,Psoralea corylifolia L. andSorphora angustifolia Sieb. & Zucc.) were selected for further study in lard held at 75°C for 7 d. The methanol extracts ofP. corylifolia L. andS. angustifolia Sieb. & Zucc. greatly decreased the peroxide formation of lard during storage. Treatment with 0.20% methanolic extract ofP. corylifolia L. exhibited significantly stronger antioxidant effect on the oxidation of lard than treatment with 0.02% butylated hydroxyanisole (P<0.05).