HPLC法测定杜仲中维生素K1

为检测杜仲中维生素K1含量,采用了特异性强、分离效果好的高效液相色谱(HPLC)法,将样品经丙酮、石油醚提取,用失活磷酸盐处理过的氧化铝进行柱色谱净化处理,用极性不同的洗脱液将维生素K1从样品中分离出来,收集V(石油醚) V(乙醚)=97 3洗脱组分,浓缩定容,用C18色谱柱对维生素K1进行定性定量分析,流动相为V(甲醇) V(正己烷)=75 25,紫外检测波长为248 nm。结果表明,在流量为1.5 mL/min的条件下,维生素K1的保留时间为(2.18±0.1)min,r为0.999 3,回收率87.67%~95.12%,杜仲中的维生素K1含量为12.404 3μg/g。     

反相高效液相色谱法同时分离测定杜仲雄花及其产品中的 京尼平苷酸和绿原酸

建立了利用反相高效液相色谱法（RP-HPLC）同时测定杜仲雄花及其产品中京尼平苷酸和绿原酸的方法。所用的色谱柱为Shim-pack VP-ODS(150 mm×4.6 mm,5 μm),流动相组成为甲醇-水-乙酸(体积比为24∶75∶1),检测波长为240 nm。在该色谱条件下,京尼平苷酸的含量在0.025~0.400 g/L、绿原酸的含量在0.075~1.200 g/L范围内线性关系良好,相关系数分别为0.9997和0.9999;加标回收率分别为100.2%和100.5%。该法适用于杜仲雄花及其产品中这2种成分的含量分析。     

Facile fabrication of a superhydrophobic surface from natural Eucommia rubber

In this study, we introduce a fabrication method for a superhydrophobic surface made from natural Eucommia rubber. Based on the Eucommia rubber extract solution, we prepared a type of superhydrophobic material using the simple phase separation method and the addition of a low‐surface‐energy substance method, thus developing a new approach for the application of natural Eucommia rubber. The experimental results showed that a superhydrophobic film could be obtained by both the addition of acetone and induction by water vapor. Additionally, the film exhibited properties closely related to the crystalline Eucommia rubber spherical particles with a hierarchical structure. The addition of hydrophobic silica also increased the hydrophobic property of the Eucommia rubber film. When the content of the silica was 4% (wt%), the contact angle of the composite film reached 160.7°, which could be attributed to the properties of the nano‐silica and the micro‐nano structure of the composites. Copyright © 2017 John Wiley & Sons, Ltd.     

高效液相色谱法测定杜仲中京尼平甙酸

ODS- C18色谱柱 (2 0 0 mm× 4 .6 mm,5 μm) ,甲醇 -水 -冰乙酸 (12∶ 87∶ 1)为流动相 ,高效液相色谱法测定了杜仲中京尼平甙酸的含量 ,考察了流动相组成、酸性添加剂对色谱分离效果的影响 ,流速 1.0 m L/ min时 ,京尼平甙酸的容量因子 k′在 2— 3之间 ,分离度大于 1,保留时间为 6 .9min,样品分析时间在 30 min之内 ,满足色谱分析要求。京尼平甙酸在 0 .0 36— 1.36 mg/ m L时 ,色谱峰面积与样品量呈良好的线性关系 ,线性方程为 A=6 375 6 132 72 6 0 C,相关系数 r=0 .9996。     

Focused microwave-assisted solvent extraction and HPLC determination of effective constituents in Eucommia ulmodies Oliv. (E. ulmodies)

A new focused microwave-assisted solvent extraction method using water as solvent has been developed for leaching geniposidic and chlorogenic acids from Eucommia ulmodies Oliv. The extraction procedures were optimized using a two indexes orthogonal experimental design and graphical analysis, by varying irradiation time, solvent volume, solvent composition and microwave power. The optimum extraction conditions were obtained: for geniposidic acid, 50% micorwave power, 40 s irradiation, and 80% (v/v) aqueous methanol as extraction solvent (20 ml g⁻¹ sample); and for chlorogenic acid, 50% micorwave power, 30 s irradiation, and 20% aqueous methanol (20 ml g⁻¹ sample). The composition of the extraction solvent was optimized and can be directly used as the mobile phase in the HPLC separation. Quantification of organic acids was done by HPLC at room temperature using Spherigel C₁₈ chromatographic column (, i.d. 5 μm), the methanol:water:acetic acid (20:80:1.0, v/v) mobile phase and UV detection at 240 nm. The R.S.D. of the extraction process for geniposidic and chlorogenic acid were 3.8 and 4.1%, respectively.     

杜仲叶中绿原酸提取分离工艺条件的研究

对杜仲叶绿原酸的提取分离进行研究.探讨了水以及不同浓度乙醇、甲醇和丙酮水溶液作为提取溶剂对绿原酸得率的影响,采用正交实验方法对影响绿原酸提取率的主要因素进行分析,并采用大孔树脂对其分离.结果表明,50℃水提绿原酸得率比较高,其得率为1.06%,从而确定水作为绿原酸提取溶剂;水提杜仲叶绿原酸的最佳工艺条件为:温度60℃,料液比1∶16,pH4,提取时间3h,所筛选的GC-I树脂是吸附分离绿原酸的最佳吸附剂,吸附最佳pH值为3,吸附流速为3BV/h;本实验条件下得到粗产品纯度为30.88%,收率为76.51%.     

Metabolomics comparison of chemical components and metabolic regulations in different parts of Eucommia ulmoides Oliv

Eucommia ulmoides Oliv. (EU) is an herb with variety of pharmacological activities. As the demand for EU as a medical source increases, its limited availability is becoming an urgent problem. The bark of EU—Eucommia cortex (EC)—was the main medicinal part of EU, whose yield has been too low to meet market requirements. The EU leaves—Eucommiae folium (EF)—obtained easily from the trees, traditionally considered less valuable than the EU bark. This study compared chemical components and metabolic regulations in different parts of EU using metabolomics to explore the potential for alternative medical sources of EU. The results demonstrated that the composition of EC differs slightly from the composition of EF, and there are some differences in the content of individual ingredients between EC and EF. Combined pharmacodynamic/metabolomics analysis showed that both EC and EF could improve the bone metabolism markers and trabecular microarchitecture of ovariectomized rats mainly by intervening in amino acid metabolism. Our data suggest that EF is a potential alternative medicinal option when EU resources are scarce, and this study provides a mechanistic framework for the benefits of EF in osteoporosis disease.     

原子荧光光谱法测定杜仲中的砷

采用双通道原子荧光光谱法测定杜仲中砷的含量。确定了仪器的最佳工作条件,考察了酸度、还原剂、预还原剂的影响以及共存元素的干扰情况。方法快速、简便、准确且灵敏度高,为中药材中砷的含量测定提供了较好的方法。     

陕西略阳杜仲叶中绿原酸的含量分析

测定了陕西略阳杜仲叶中绿原酸的含量,为陕西略阳杜仲产业发展提供基础研究数据和分析技术支持。采用微波提取,设置微波功率200W,压力1000kPa,温度60℃,提取5min;高效液相色谱法分析检测,设置色谱条件为Diamonsil C18柱(4.6mm×150mm,5μm),327nm检测波长,流动相为乙腈∶0.3%磷酸=15∶85,1mL/min流速,30℃柱温。采用微波提取法处理样品,绿原酸提取效率高;HPLC分析方法通过方法学考察符合分析要求;陕西略阳杜仲叶中绿原酸含量在1.85%—3.18%之间。陕西略阳杜仲叶中绿原酸的含量远高于药典要求,可单独作为药材使用,亦可作为绿原酸提取原料使用,具开发利用价值。     

杜仲内生真菌抗氧化活性

应用TBA反应法对从杜仲(Eucommia ulmoides Olive．)叶片中分离到的内生真菌刺孢壳Chaetomella sp．培养液提取物进行的抗氧化活性的测定表明该菌能够产生抗氧化活性成分，通过TLC和HPLC对抗氧化活性成分的分析表明其活性成分为黄酮类化合物。