The study on determination of trace elements and transference characteristics in the botanic chinese medicinal herb of reducing blood sugar and health food

目的 :对植物性降血糖中药及保健食品中微量元素的含量及溶出特性进行研究 ;方法 :电感耦合等离子体质谱法 (ICP -MS) ;结果 :不同的降血糖中药和保健食品的消解液及冲泡液中锰、铁、锌、钙的含量都很高 ,铜、镍、硒次之 ;其中BCBT茶中镍的溶出率最高达 6 0 2 % ,铜、锌次之 ,分别为 38 7%、35 1%。objective: studying the determination of trace elements and transference characteristics in the botanic chinese medicinal herb of reducing blood sugar and health food; methods: Inductively Coupled Plasma Mass Spectrometry(ICP-MS); results: in different chinese medicinal herbs of reducing blood sugar and health food ,the contents of Mn?Fe?Zn?Ca are very high, followed by Cu?Ni?Se and the extractive content of Ni in BCBT tea is the highest :60 2% ,Cu Zn is second: 38 7%?35 1%.福建省青年科技人才创新项目 ( 2 0 0 1J0 63

Determination of Salvianolic acid B by High Performance Liquid Chromatography with Fluorescence Detection

建立了丹酚酸B的高效液相色谱-荧光检测含量测定方法。色谱条件为:BACKMANODS柱( 4 6mmi.d .×2 5 0mm ,5 μm) ,以甲醇-0 5 %冰醋酸水溶液为流动相,流速为1 0mL/min ;荧光检测波长λEX=3 3 8nm ,λEM=44 3nm ;进样量5 μL。丹酚酸B进样量为0 12～1 2 μg时,其质量与峰面积呈良好的线性关系(r=0 9998) ;加样回收率为98 6%～10 8% ;最低检测限为0 0 13 μg/mL。该法具有更高的灵敏度,为丹酚酸B的药代动力学研究提供基础A new method for the determination of Salvianolic acid B by high performance liquid chromatography with fluorescence detection has been established.The column used was BACKMAN C 18 (4.6mm i.d.×250mm,5μm);The mobile phase was methanol-0.5% acetic acid solution with gradient condition at a flow rate of 1.0mL/min;The fluorescence detector was operated at λ EX =338nm and λ EM =443nm with the injection volume of 5μL.The result proved that Salvianolic acid B has a good linearity in the range of 0.12μg to 1.2μg with the correlation coefficient of 0.9998;The recoveries were 98.6%～108%;The limit of detection is 0.013μg/mL.This method has a higher sensitivity and can be used in the study of pharmic metabolize.国家自然科学基金重点项目(2 0 2 350 2 0

Study on the Preparation of Salvianolic Acid B of High Purity

目的:建立高纯度丹酚酸B的最佳制备工艺流程。方法:通过比较几种不同大孔吸附树脂对丹酚酸B的吸附及洗脱性能,筛选出最佳树脂并对该树脂分离纯化丹酚酸B的工艺参数进行优化。结果:在本文所确定的最佳工艺条件下,丹酚酸B回收率为90.6%,纯度高达91.8%,稳定性良好,可作为丹参制剂的原料药应用。结论:该工艺操作简便,适用于工业化生产,有利于促进丹酚酸B的开发利用。Objective:The best technology of the preparation of salvianolic acid B was established.Methods:A series of macroporous adsorption resins were compared on their adsorption and desorption properties for salvianolic acid B and the optimal type resin had been selected. The technical parameters for purification of salvianolic acid B with the selected type resin were studied. Results:Under this condition, the recovery is 90.6% and the purity of salvianolic acid B is 91.8%. The product has a good stability and could be used for preparation directly.Conclusion:This method is simple and could be used for industrial production, promoting the exploitation and utilization of salvianolic acid B.国家自然科学基金重点项目(No.20235020);; 青岛市重点实验室建设项目(No.04-2-JS-135

Preparative Separation of Salvianolic Acid B from Salvia miltiorrhiza by High Speed Counter-Current Chromatorgraphy

采用高速逆流色谱法分离纯化丹参水溶性成分丹酚酸类物质,制备丹酚酸B化学对照品。分离采用的溶剂系统为正己烷-乙酸乙酯-水-甲醇(1.5:5:5:1.5),上相做固定相,下相做流动相,流速为1.7 mL/min,仪器转速850 rpm,进样量80 mg,纯度用HPLC方法测定。结果表明:一次分离可制备63.4 mg丹酚酸B,其纯度为98.6%。该方法操作简单,可作为高纯度丹酚酸B化学对照品的制备分离方法。Salvianolic acid B,a major bioactive component in Danshen(Salvia miltiorrhiza Bge.),was isolated and purified by high-speed counter-current chromatography(HSCCC) in semi-preparative scale from the crude extract of Danshen.Separation was performed with a two-phase solvent system composed of hexane-ethyl acetate-water-methanol(1.5:5:5:1.5,v/v) by eluting the lower aqueous phase at a flow-rate of 1.7 mL/min and a revolution speed of 850 rpm with injection volume of 80 mg.After the proceeding of separation,63.4 mg salvianolic acid B was obtained,and analyzed by normalization method according to HPLC areas giving a purity of 98.6%.HSCCC is a recommendable method to prepare and purify the active constituents from Salvia miltiorrhiza.国家自然科学基金重点项目(20235020);; 厦门市科技创新重点项目(3502Z20031096

Classification of Panax Quinquefolium.L Samples by Cluster Analysis

建立西洋参药材分类方法;分别采用电感耦合等离子体质谱(ICP-MS)法、高效液相色谱(HPLC)法以及蒽酮-硫酸分光光度法,对12个西洋参样品中的15种无机元素、7种人参皂苷和多糖进行测定,用SPSS聚类分析法对12个西洋参样品进行聚类分析;结果表明:以4种不同的聚类变量进行聚类分析,其聚类分组结果并不一致,将几种有效成分综合为聚类变量,对西洋参进行分类更为科学合理;聚类分析法是西洋参分类分析的有效方法,对西洋参品种与质量的鉴定有一定的理论意义和实用价值。A classification method was developed for the quality assessment of Panax Quinquefolium.L.The contents of fifteen elements,seven ginsenosides and polysaccharide in twelve Panax Quinquefolium.L samples were determined by ICP-MS,HPLC and anthrone-sulfuric acid spectrophotometry,respectively.The cluster analysis was applied for the classification of 12 Panax Quinquefolium.L samples.The analysis results showed that the classified results were different with different cluster variables and it was found more reasonable to integrate several active components as cluster variables for the classification.The cluster analysis was useful for the classification of Panax Quinquefolium.L

苯胺基喹唑啉类酪氨酸激酶抑制剂的电喷雾质谱裂解规律

研究吉非替尼、厄洛替尼和艾克替尼3种苯胺基喹唑啉类酪氨酸激酶抑制剂,在电喷雾质谱正离子模式下的裂解规律.通过电喷雾质谱产生各化合物稳定的[M+H]+准分子离子峰,进而对[M+H]+离子进行高能诱导裂解和碰撞诱导裂解,获得相应化合物的质谱图.结果表明:在电喷雾电离（ESI）多级质谱中,3种药物的裂解主要发生在喹唑啉环C4,C6和C7位取代基上,并伴随分子内重排和H+的迁移重排;在二级质谱图中,吉非替尼的高丰度特征离子质荷比（m/z）为128.1,厄洛替尼的m/z值为278.1和336.1,埃克替尼的m/z值为278.1,304.1.国家自然科学基金资助项目(81302652);;福建省自然科学基金资助项目(2015J01342

贝壳吸声界面吸声性能试验研究

以贝壳、玻璃棉为主要材料,利用贝壳、玻璃棉、空腔组成一个吸声界面,通过驻波管吸声降噪的试验研究,探究不同厚度的贝壳层、玻璃棉层、空腔这三者的搭配组成的吸声界面的吸声频谱特性及变化规律,用于不同贝壳层厚度、不同玻璃棉厚度吸声性能的预测评估,为最终实现贝壳吸声产品研发提供参考

4-氨基苯甲酸对蘑菇酪氨酸酶的抑制作用机理研究

报道了4-氨基苯甲酸(4-aminobenzoic acid)对蘑菇酪氨酸酶单酚酶和二酚酶活力的影响和抑制效应.结果表明,4-氨基苯甲酸对蘑菇酪氨酸酶的单酚酶和二酚酶活性均有抑制作用.导致单酚酶活力和二酚酶活力下降50%的抑制剂浓度(IC50)分别为0.35和0.30 mmol/L.4-氨基苯甲酸对单酚酶的迟滞时间有明显的延长效应,1.0 mmol/L可使单酚酶的迟滞时间从30.5 s延长到155.1 s,增加了4.4倍.4-氨基苯甲酸对二酚酶的抑制作用表现为混合型可逆抑制作用,抑制常数(KI和KIS)分别为0.259和1.46 mmol/L