Simultaneous determination of saponins in Radix Glycyrrhizae, Notoginseng and Ginseng by high performance liquid chromatography

To establish a method for determining five saponins（notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate） in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector（HPLC-DAD） method was applied to an Inertsil ODS-SP column（4.6 mm×250 mm, 5 μm） with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1（r=1.000,0）, 0.751,1— 7.511,4 μg for Rg1（r=1.000,0）, 0.677,2—6.771,6 μg for Re（r=1.000,0）, 0.733,9—7.339,1 μg for Rb1（r= 1.000,0）, and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate（r=0.999,9）, respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations（RSDs） of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.     

反相高效液相色谱法测定慈姑中的几种酚类组分

通过实验建立了慈姑中愈创木酚、儿茶酚、焦性没食子酸的含量测定方法,该测定方法快捷、简便、准确,所测结果稳定、重现性好。实验采用ODS柱,柱温35℃,甲醇-水（含1%乙酸,体积比为35：65）溶液为流动相,用紫外检测器于275 nm处检测。结果表明,愈创木酚进样量为0.03μg~1.2μg;进样量与色谱蜂呈良好的线性关系（r=0.998）;样品的加标回收率为98%~101%;相对标准偏差（RSD）为1.40%（n=6）。     

Mathematical model of the dynamics of countercurrent chromatography

A mathematical model of the dynamic behavior of countercurrent chromatography was proposed, and the model parameters, including the partition coefficient, the axial dispersion coefficient, the intraparticle diffusion coefficient and the external mass ransfer coefficient were calculated by the method of chromatogram moment analysis. Comparison of the experimental chromatograms of caffeine and theophylline determined in this work with the simulated curves computed by the proposed model showed fairly good agreement. Further, the difference between the average identified the partition coefficients by chromatogram moment analysis and the experimental values was small also, and the relationship between the external mass transfer rate and the linear velocity was similar to that obtained with solid-liquid chromatography.     

Isolation ofMycobacterium Tuberculosis 31 kDa antigen protein of diagnostic interest from culture filtrate using anti-ES-31 antibody by affinity chromatography

Proteins secreted into the culture medium byMycobacterium tuberculosis (M. tb) are shown to be source of antigens of immunodiagnostic interest. Anin vitro released 31 kDa antigen ESAS-7F isolated fromM.tb H₃₇Ra culture filtrate by salt precipitation, SDS-PAGE and cation exchange fast protein liquid chromatography (FPLC) was shown earlier to be a diagnostically important antigen fraction. In this report, we describe the isolation of ESAS-7F antigen using monospecific antibody coupled to sepharose CL-4B column. The percentage recovery of ESAS-7F antigen using affinity chromatography was approximately 8% of the total ES antigen proteins compared to 0.05% obtained by conventional purification steps using salt precipitation, SDS-PAGE and FPLC. Similar seroreactivity was observed by the antigen isolated by both the methods in indirect ELISA. Affinity chromatography helped in an increased recovery of ESAS-7F antigen and obviates the need for time consuming conventional purification steps.     

以滑移机理探讨色谱分析的塔板数

以滑移色谱机理弥补塔板理论的不足，滑移色谱机理的色谱流出曲线函数可更真实地表达实际色谱流出曲线。在计算色谱柱塔板数时，应区分色谱柱塔板数和色谱峰塔板数（是由实际色谱峰形得到的，在色谱过程中实际发生的），因色谱柱塔板数与色谱峰塔板数是不同的概念。推导出色谱拄塔板数与色谱峰塔板数之间的关系式。该关系式成功地解释了通常色谱峰显著拖尾的原因。丙酮在GDX-101上的吸附焓△H=-3.6k．J／mol.     

离子对液相色谱在医学分析中的应用

综述了正、反相离子对液相色谱法在临床、药物等医学分析中的应用，引用献14篇．     

薄层色谱分离—紫外光度法测定稻瘟灵主成份

本文研究了以硅胶G为吸附剂的薄层色谱法从农药稻瘟灵原油或乳油中分离出主成份1,3—二硫戊环—2—叉—丙二酸二异丙酯(DIDM)的最佳条件,拟定了用紫外分光光度法测定样品中DIDM含量的实用的新方法.     

气相色谱法测定面粉中过氧化苯甲酰

面粉中的过氧化苯甲酰经乙醚提取浓缩后,被碘化钾还原反应生成苯甲酸,利用气相色谱法对其进行分离测定,并与标准品比较定性、定量.该方法的最低检出含量为0.3 mg/kg,加标回收率在90%～99%之间.该方法分离效率高,样品用量少,检测灵敏度高.     

A novel long-chain acyl-derivative of epigallocatechin-3-O-gallate prepared and purified from green tea polyphenols

Lipophilic tea polyphenols (LTP) were prepared by catalytic esterification of green tea polyphenols (GTP) with hexadecanoyl chloride. A novel long-chain acyl-derivative of epigallocatechin-3-o-gallate (EGCG) was first isolated from purification of LTP by high-speed countercurrent chromatography (HSCCC) using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1∶1∶1∶1, v/v). The molecular structure of the acyl-derivative, Epigallocatechin-3-O-gallate-4′-O-hexadecanate, was elucidated by means of elemental analysis, IR,¹H-NMR and MS spectra. Project (No. 200010) supported by Zhejiang Provincial Natural Science Foundation, China