制备型高效液相色谱已广泛应用于医药、精细化工、食品等行业,特别适用于分离高附加值、高纯度的产品。通过制备型高效液相色谱分离生育酚各组分的教学实践,探讨了制备型高效液相色谱实验教学内容的设置,以及通过实验教学提高学生独立分析和解决问题能力的方法,强化了学生的应用能力。

Preparative high performance liquid chromatography has been widely applied in medicine, fine chemical and food, particu- larly applicable to separate high added value and high purity products. Tbis paper introduced the experiment teaching of preparative high performance liquid chromatography in separation of tocopherol, explored how to set up teaching content, and the ways of improving students ＂abilities to analyze and solve problems. The stvdents＇application abilities were strengthened.

研究了制备型高效液相色谱分离纯化女贞子中红景天苷的方法。制备色谱的参数为：色谱柱为C18柱（50 mm ×200 mm,5μm）,流动相为甲醇-水（体积比为7．5∶92．5）,流速100 mL·min-1,二级管阵列检测器在278 nm检测,进样体积为2．2 mL。在18 min的运行时间内,红景天苷与干扰成分得到很好的分离,经HPLC检测纯度均达到98%以上。此方法具有快速高效、分离组分纯度高的特点,可用于制备红景天苷。

The objective of this study is to develop a preparative high performance liquid chromatography( HPLC) method for the iso-lation and preparation of salidroside from Ligustrum lucidum. The optimum operation parameters were selected as follows a C18 col-umn(50 mm × 200 mm,5 μm)with methanol-water(7. 5∶92. 5,V/V)as the mobile phase at a flow rate of 100 mL/min,the detec-tion wavelength of 278 nm,and the injection volume of 2. 2 mL. Salidroside can be obtained in 18 min,and the purities of the prod-ucts were detected by HPLC method. The results displayed that the purities of products were above 98%. The effective and rapid method has been successfully applied to the preparation of salidroside from Ligustrum lucidum.

目的研究大黄藤(Fibraurea Recisa Pierre)中的化学成分.方法利用正相硅胶柱色谱、半制备型高效液相色谱、葡聚糖凝胶及反相中压液相色谱等现代分离技术进行分离,根据理化性质和NMR,MS等方法鉴定其结构.结果从中分离得到8个化合物,分别是黄藤内酯(1),马克甾酮A(2),环阿屯醇(3),feruloylphenethylamine(4),反式阿魏酰酪胺(5),β-谷甾醇(6),1-棕榈酸单甘油酯(7),1-sinapoyl-β-D-glucopyranoside(8).结论化合物2~8为首次从该植物中分离得到.

Objective The purpose of this study was to investigate the chemical constituents of Pierre. Methods The chemical compositions were isolated by silica gel column chromatography, semi-preparative HPLC,Sephadex LH-20, and MPLC packed with MCI gel, and their structures were identified on the basis of chemical and spectroscopic evidence (NMR and MS) . Results Eight compounds were obtained and determined as fibraurin (1),makisterone A (2),cycloartenol (3),feruloylphenethylamine (4),trans- -feruloyltyramine(5),β-sitosterol(6),1-monopalmitin(7),1-sinapoyl-β-D-glucopyranoside(8). Conclusion Compounds 2-8 were isolated from this plant for the first time.

目的 研究翠柏(Calocedrus macrolepis)中的倍半萜成分.方法 利用正相硅胶柱色谱、半制备型高效液相色谱、葡聚糖凝胶及反相中压液相色谱等现代分离技术进行分离,并根据化合物的物理特性及波谱信息鉴定其结构.结果 从中分离到4个倍半萜和1个酚类化合物,分别是caryolane-1,9β-diol(1),eudesma-4(15)-ene-lβ,6α-diol(2),5-epi-eudesma-4(15)-ene-1β,6 β-diol(3),eudesma-11(13)-ene-4β,9β-diol(4),coniferaldehyde (5).结论 4个倍半萜和1个酚类化合物均为首次从翠柏中分离得到.

Objective To study the chemical compositions of Calocedrus macrolepis.Methods The chemical compositions were isolated with silica gel column chromatography, semi-preparative HPLC, Sephadex LH-20 and MPLC packed with MCI gel and their structures were elucidated on the basis of physical characteristics and spectral data. Results Five compounds were obtained, and their structures were identified as caryolane-1, 9β-diol (1),eudesma-4(15)-ene-lβ,6α-diol (2),5-epi-eudesma-4 (15)-ene-1β,6β-diol (3), eudesma-11(13)-ene-4β,9β-diol (4), coniferaldehyde(5). Conclusion All of these compounds are isolated from the Calocedrus macrolepis for the first time.

目的比较反流安无糖型混悬颗粒不同制备工艺制剂质量,确定最佳制备工艺。方法对水提、醇提2种工艺按不同制粒配方制备的颗粒色泽、均匀度、味道、气味进行比较,确定浓浸膏-木糖醇-糊精的比例,并对颗粒的溶化性、粒度、流动性进行考察。分别采用薄层色谱法鉴别2种工艺制备的颗粒中的柴胡、白芍、枳实、延胡索,采用高效液相色谱法测定芍药苷和橙皮苷的含量,对水提和醇提效果进行比较。结果反流安无糖型混悬颗粒最佳制备工艺为:柴胡、枳实、白芍、甘草加12倍量80%乙醇浸泡30 min,提取1.5 h,药渣与生姜、竹茹、蒲公英、延胡索加8倍量水,提取2次,每次1.5 h,滤过,合并3次滤液,浓缩至膏状,按浓浸膏∶木糖醇∶糊精=1∶1∶3进行制粒。结论该方法操作简单,稳定,可行。

Objective To compare the quality of Free-sugar Suspended Granules of Fanliuan of different preparation technology, and optimize its preparation process. Methods The color, uniformity, taste and smell of particles of two kinds of extraction process were compared to optimize the proportion of drug, xylitol and dextrin of particle formation process, and dissolubility, size, liquidity of particles were investigated. Bupleuri radix, Aurantii fructus immaturus, Paeoniae radix alba and Rhizoma corydalis were identified by TLC, and paeoniflorin and hesperidin were determined by HPLC to compare the effect of water extraction and alcohol extraction. Results The best preparation process was as follows:Bupleuri radix, Aurantii fructus immaturus, Paeoniae radix alba and Glycyrrhizae radix et rhizoma were soaked with 12 times amount of 80%ethanol for 30 min, extracted for an hour and a half. Then the extract dreg and Zingiber officinale Rosc, Bamboo shavings, Taraxacum mongolicum, Corydalis rhizoma