Preparative isolation and purification of 12,13-dihydroxyeuparin from Radix Eupatorii Chinensis by high-speed counter-current chromatography

An efficient method for the isolation and purification of 12,13-dihydroxyeuparin from Radix Eupatorii Chinensis by high speed counter-current chromatography (HSCCC) was established in this paper. The ether extracts of Radix Eupatorii Chinensis were purified by HSCCC with a solvent system of hexyl hydride-ethyl acetate-methanol-water (1:2:1:2, v/v/v/v). The upper phase was used as the stationary phase and the lower phase as the mobile phase. About 8.4 mg of 12, 13-dihydroxyeuparin was obtained from 200 mg of ether extracts from Radix Eupatorii Chinensis in one-step HSCCC separation, with the purity of 96.71%, as determined by HPLC. After methanol- water recrystallization, the purity of 12,13-dihydroxyeuparin reached 99.83%. Such a simple and effective method was fairly useful to prepare pure compound as reference substances for related study on Radix Eupatorii Chinensis.

Preparative separation and purification of deoxyschizandrin from Schisandrae Sphenantherae Fructus by high-speed counter-current chromatography

A high-speed counter-current chromatography （HSCCC） method was successfully developed for the preparative separation and purification of deoxyschizandrin from Schisandrae Sphenantherae Fructus in one step. The purity of deoxyschizandrin was 98.5%, and the structure was identified by MS, UV and NMR. This method was simple, fast, convenient and appropriate to prepare pure compound as reference substances for related research on Schisandrae Sphenantherae Fmctus.

An Economical Method for Preparative Purification of Five Alkaloids from Coptis Chinensis Franch by High-Speed Counter-Current Chromatography Using Singled Prepared Solvent System by GC

Coptis chinensis Franch, a widely used Traditional Chinese Medicine, shows various kinds of bioactivity. The major active components of the herb are considered to be alkaloids. Thus, preparative separation of these alkaloids is critical important for further pharmacology and mechanism studies. In the paper, five alkaloids from C. chinensis were purified by HSCCC using the solvent system composed of chloro-form-metha- nol-water (2:1:1, v/v/v) single prepared. The content of each solvent in solvent system were determined by gas chromatography (GC), then according the ratios of solvents in each phase to prepare the mobile and stationary phase respectively. And a comparative study was carried out between together preparation and single preparation of the solvent system. The purities and recoveries of all the products were over 98.5% and 92%. However, 134 mL chloroform, 336 mL methanol and 452 mL water were saved when the two phase were singled by GC. Our research showed an economical method for separating alkaloids from C. chinensis by HSCCC using the solvent system single prepared by GC.

Separation and Purification of Acetophenones from Cynanchum bengei Decne Root Bark by Combination of Silica Gel and High-speed Counter-current Chromatography

[Objectives] To develop a method for separation and purification of acetophenones from Cynanchum bengei Decne root bark by combination of silica gel and high-speed counter-current chromatography( HSCCC). [Methods]The crude extract of Cynanchum bengei Decne root bark was separated by silica gel column chromatography,and parts A and B containing acetophenones were obtained. Then,parts A and B were separated by HSCCC with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water( 4∶ 6∶ 4. 5∶ 5. 5 and4∶ 6 ∶ 3 ∶ 7, V/V), respectively. [Results] From 260 mg of part A, four compounds with p-dihydroxybenzene 3. 9 mg(Ⅰ),4-hydroxyacetophenone 17. 1 mg( Ⅱ),2,5-di-hydroxyacetophenone 13. 3 mg(Ⅲ) and 2,4-dihydroxyaceto-phenone 21. 0 mg(Ⅳ) were obtained. And from 300 mg of part B,136 mg of Radix Cynanchi Bungei benzophenone(Ⅴ) was obtained. The purity of compounds determined by HPLC was 97. 0%,96. 6%,99. 2%,99. 7%,99. 5%,respectively. [Conclusions] The established method is simple and efficient. It can be used for separation of acetophenones from Cynanchum bengei Decne root bark and has better practical value,which could provide a reference basis for development and utilization of Cynanchum bengei Decne root bark.

猪苓中黄嘌呤氧化酶抑制剂的筛选分离及质谱分析

试验以猪苓为研究对象,综合利用遗传算法-BP神经网络数学模型、色谱和质谱等技术,建立快速筛选猪苓中黄嘌呤氧化酶抑制剂的新方法。首先,利用遗传算法-BP神经网络数学模型优化猪苓中麦角甾醇的提取工艺;其次,以黄嘌呤氧化酶为生物靶分子,应用超滤质谱技术,筛选猪苓中潜在的黄嘌呤氧化酶抑制剂,同时,应用分子对接技术验证超滤实验的准确性;最后,以活性筛选为导向,利用高速逆流色谱技术分离猪苓中黄嘌呤氧化酶抑制剂。结果显示:猪苓中麦角甾醇的最佳提取工艺为乙醇体积分数80%、液料比16 mL/g、提取时间1.4 h、提取次数3次,在此条件下,麦角甾醇得率为2.31%;从猪苓中筛选并分离出4个纯度均在90%以上的黄嘌呤氧化酶抑制剂,其抑制效果强弱顺序为猪苓酮A>猪苓酮B>麦角甾-4,6,8(14),22-四烯-3-酮>麦角甾-7,22-二烯-3-酮。该方法快速、灵敏,为猪苓抗痛风药理作用的进一步研究提供了一定的理论基础。

活性引导结合高速逆流色谱分离蓝莓活性成分及其与α-葡萄糖苷酶的相互作用

基于活性引导结合高速逆流色谱(HSCCC)技术,分离蓝莓中具有抑制α-葡萄糖苷酶活性的组分。首先,经不同溶剂提取后,活性成分在水中得到富集;其次,通过HSCCC分离水提物,得到6种组分,其中F4对α-葡萄糖苷酶的抑制率显著高于其它几种;再次将F4采用Sephadex LH-20葡聚糖凝胶纯化,得到高纯的组分Ⅰ;最后通过紫外光谱、傅里叶红外光谱、高效液相色谱-质谱联用及核磁技术鉴定组分Ⅰ为矢车菊-3-O-葡萄糖苷(C3G),纯度为95.06%。此外,采用多光谱扫描和分子对接技术对C3G与α-葡萄糖苷酶的相互作用进行表征。研究发现C3G与α-葡萄糖苷酶通过氢键自发结合形成复合物。与C3G复合后,α-葡萄糖苷酶的二级结构发生不同程度的变化,其中α-螺旋和β-转角降低,β-折叠和不规则卷曲增加。分子对接模拟发现C3G与残基Leu 313、Ser 157、Tyr 158、Phe 314、Arg 315和Asp 307以氢键结合,并与周围4个疏水残基存在疏水作用,共同维持复合物结构。本研究结果对开发2型糖尿病功能性食品具有重要意义。

Isolation and Purification of Isoaloeresin D and Aloin from Aloe vera by High-speed Counter-current Chromatography

Objective To develop an efficient method to isolate and purify the main components isoaloeresin D and aloin from Aloe vera for its industrial production.Methods High-speed counter-current chromatography was used to isolate isoaloeresin D and aloin in a one-step separation from dried crude extract of A.vera.The biphasic solvent system composed of hexane-ethyl acetate-acetone-water(0.2:5:1.5:5) was used at a flow rate of 1.0 mL/min,while the lipophilic phase was selected as the mobile phase and the apparatus was rotated at 840 r/min.The effluent was detected at 254 nm.Results Isoaloeresin D(53.1 mg) and aloin(106.9 mg) were separated from the crude extract(384.7 mg) with the purities of 98.6% and 99.5%,respectively.Conclusion HSCCC is a powerful technique for isolation and separation of chemical composition from aloe.

Separation of Five Quinolone Alkaloids from Fruits of Evodia rutaecarpa by High-speed Counter-current Chromatography

Objective To develop a suitable method for the large-scale separation of quinolone alkaloids from the fruits of Evodia rutaecarpa by high-speed counter-current chromatography （HSCCC）. Methods Two solvent systems were developed for the separation method. The upper phase was used as the stationary phase, and the lower phase was used as the mobile phase at 35 oCwith the flow rate of 2 mL/min and rotation speed of 855 r/min. Results Using the described method, 1-methyl-2-undecyl- 4（1H）-quinoione （1）, evocarpine （2）, 1-methy-2-[（6Z,9Z}]-6,9-pentade-cadienyl-4- （1H）-quinolone （3）, dihydroevocarpine （4）, and the mixture （5） of 1-methyl-2-[（z^- 10-pentadecenyl]-4（1H）-quinolone （Va） and 1 -methyl-2-[（Z^-6-pentadecenyl]- 4（1H）-quinolone （Vb） could be isolated from a petroleum ether extract. They were identified by 1H-NMR, ~3C-NMR, and MS/MS, and the purities were 94.3%, 95.2%, 96.8%, 98.3%, and 96.8%, respectively. Conclusion Five quinolone alkaloids from the fruits of E. rutaecarpa could be systematically isolated and purified using HSCCC. The presented method is simple and efficient with good potentials on the preparation of reference substances, especially on the quality control of Chinese materia medica.

Preparative Separation of Four Alkaloids from Gelsemium elegans by High-speed Counter-current Chromatography

Objective To develop an efficient preparative method for the separation of Gelsemium alkaloids from Gelsemium elegans. Methods High-speed counter-current chromatography （HSCCC） with several two-phase solvent systems was investigated for the separation of Gelsemium alkaloids. The purity and structure identification of the purified compounds were performed with HPLC and NMR spectra, respectively. Results In a single operation, 206.6 mg of crude alkaloid sample was separated to yield 28.7 mg of koumine, 24.9 mg of gelsemine, 26.9 mg of humantenine, and 7.2 mg of gelsevirine, with the purities of 97.8%, 95.4%, 97.4%, and 93.5%, respectively. Conclusion A preparative HSCCC method is successfully established for the separation of four Gelsemium alkaloids from G. elegans with a modified two-phase solvent system com posed of n-hexane-ethyl acetate-ethanol-O. 5% triethylamine-H2O （3：5：3：4）.

物料视觉分拣系统的研究与开发

【目的】物料分拣是工农业生产不可或缺的环节,机械化分拣不仅能够节约成本、提高工作效率,而且能够提高分拣的准确率。【方法】笔者设计了一套简单、高效且低成本的自动分拣系统,分析了系统的硬件结构和软件结构。笔者选用西门子S7-1200PLC作为该物料视觉分拣系统的控制核心,综合运用视觉控制器、变频器、编码器、电磁阀组、传感器、高速计数器、三相异步电机、气缸等设备,以亚龙YL-36A自动化装置为控制对象,进行系统调试。【结果】该系统能够对物料颜色及形状进行识别,实现对不同颜色物料的自动分拣,并且可以通过人机界面进行实时参数监测、手动调试或自动运行。【结论】该物料视觉分拣系统运行稳定,有利于改变传统的生产模式,提高生产效率,节约生产成本,经济效益显著。因此,大规模的现代化自动化物料传送与分拣,符合时代的发展趋势,值得广泛推广。

“高铁居民”实现共同富裕的“梗阻”因素——“非均衡态”高铁布局与逆城市化

如何实现全体人民共同富裕对推进“中国式现代化”至关重要。文章基于“中心—外围”城市高铁网络非均衡增密格局研究“高铁居民”共同富裕的实现路径。主要发现:第一,高铁网络增密对城市恩格尔系数存在显著倒U形影响,高铁网络增密更有利于相对富裕并且贫富差距较大城市的“高铁居民”实现共同富裕。第二,高铁网络非均衡增密会扩大“中心—外围”城市“高铁居民”贫富差距。第三,距离中心城市66.10公里范围以内的非中心城市开通高铁站有利于“高铁居民”共同富裕,距离中心城市66.10—105.76公里的非中心城市开通高铁站不利于“高铁居民”共同富裕。第四,非中心城市逆城市化是高铁网络非均衡增密拉大“中心—外围”城市“高铁居民”贫富差距的重要原因。高铁网络增密格局应从非均衡态向均衡态转变以加速“高铁居民”推进共同富裕进程。

高速逆流色谱分离与鉴定鹿药中黄酮类化合物

采用高速逆流色谱(HSCCC)与其它色谱联用的方法分离纯化鹿药中的化学成分,得到5个黄酮类化合物:5,7,3′,4′-四羟基-3-甲氧基-8-甲基黄酮(1)、8-甲基木犀草素(2)、3′-甲氧基木犀草素(3)、木犀草素(4)和槲皮素(5),它们均为首次自该种及该属植物中分离得到。HSCCC以V(氯仿):V(甲醇):V(水)=4:3:2混合液为溶剂,上相为固定相,下相为流动相,分离纯化得到3个分别含化合物1,4和5的主要部分,经HPLC检验纯度分别为98.3%,96.7%和95.3%;还有1个含有化合物2和3的较纯部分,通过SephadexLH-20柱色谱,以V(甲醇):V(水)=1:1混合液洗脱将二者分离。通过理化性质及紫外、红外、质谱、核磁等波谱分析确定化合物结构。

白花败酱草中异牡荆苷和异荭草苷的高速逆流色谱分离和制备

应用高速逆流色谱分离制备白花败酱草中的异荭草苷和异牡荆苷,以乙酸乙酯∶乙醇∶水(4∶1∶5)为两相溶剂系统,上相为固定相,下相为流动相,流速2.0 mL/m in,主机800 r/m in,检测波长254 nm。以此分离条件经一步洗脱,从300 mg白花败酱草粗提物中制备得到异荭草苷24.1 mg和异牡荆苷49.8 mg,产物纯度经HPLC检测高达98.0%,结构经UV、IR、MS1、H NMR和13C NMR鉴定,二者均为首次从败酱属植物中分离得到。

高速逆流色谱法分离茶叶中的生物碱

以氯仿－甲醇－磷酸二氢钠缓冲液（２３ｍｍｏｌ／Ｌ，ｐＨ５．６）（体积比４∶３∶２）为溶剂系统，上相为固定相，下相为移动相，从茶叶的总生物碱中分离出三个成分，其中一个是咖啡碱，一个是茶碱，另一个待定。将分离结果与ＴＬＣ分离结果相比较，证实了高速逆流色谱法的有效及实用性。

高速逆流色谱制备分离紫甘薯花色苷

采用高速逆流色谱法分离纯化紫甘薯花色苷。以正丁醇-乙酸乙酯-0.5%乙酸(3∶1∶4,V/V)为溶剂体系,上相为固定相,下相为流动相,流速2 mL/min,进样量300 mg,分离得到两种花色苷的混合物;混合物再以0.2%三氟乙酸-正丁醇-甲基叔丁基醚-乙腈(6∶5∶2∶1,V/V)为溶剂体系,上相为固定相,下相为流动相,流速1.5 mL/min,进样量100 mg,分离得到纯度分别为98.5%和96.7%的两个花色苷单体组分。通过紫外-可见光谱、质谱、核磁等技术进行结构鉴定,确定组分1为3-O-{6-O-(E)-咖啡酰-2-O-[6-O-(E)-对羟基苯甲酰-β-D-吡喃葡糖基]-β-D-吡喃葡糖苷}-[5-O-(β-D-吡喃葡糖苷)]芍药素,组分2为3-O-{6-O-(E)-咖啡酰-2-O-[6-O-(E)-阿魏酰-β-D-吡喃葡糖基]-β-D-吡喃葡糖苷}-[5-O-(β-D-吡喃葡糖苷)]芍药素。实验从450 g紫甘薯中获得63 mg组分1和48 mg组分2,为紫甘薯花色苷分离提供了高效、稳定、可靠的方法。

罗布麻中黄酮的超声波强化提取及高速逆流色谱分离纯化

本研究采用超声波强化提取罗布麻中总黄酮,选择乙醇浓度、超声功率、超声时间、料液比为因素进行正交试验优选出超声提取的最佳工艺条件:60%浓度乙醇,料液比为1:15,在300W的超声波下超声提取10min。此条件下,提取率达90%以上。将提取后的总黄酮应用高速逆流色谱进行分离纯化,两相溶剂系统为乙酸乙酯:乙醇:水:乙酸(4:1:5:0.25,V/V),进样量为150mg,得45mg纯度为98.6%的罗布麻甲素。

苦参生物碱的高速逆流色谱法制备研究——色谱参数和仪器参数的最佳化

应用新型的液液分配技术——高速逆流色谱法 (High Speed Counter- current Chromatography,HSCCC)对苦参生物碱类成分的分离制备进行探讨。选用氯仿 -磷酸 -磷酸钠缓冲液 (p H6 .2 0 )溶剂系统 ,经正交试验确定了HSCCC的最佳运行参数 ,将苦参粗提物分离得到 6个固态收集物 ,经 TL C4种不同展开系统证实其中有一个为单一组分。实验表明 ,HSCCC法是一种高效、简便的分离制备中草药有效成分纯品的新方法。

高速逆流色谱法分离纯化黄芪中的芒柄花素和毛蕊异黄酮

采用高速逆流色谱法(HSCCC),以正己烷氯仿甲醇水组成二相系统作为固定相与流动相,对黄芪的乙酸乙酯粗提物进行了分离纯化。结果发现:以正己烷氯仿甲醇水(体积比为1.5∶3∶3∶2)组成的系统可以从黄芪的乙酸乙酯粗提物中分离出毛蕊异黄酮,纯度可达95%以上,并可以初步纯化芒柄花素;接着用正己烷氯仿甲醇水(体积比为4∶4∶5∶4)组成的系统进一步纯化芒柄花素,其纯度达95%以上。利用该方法,可以对中药黄芪中的异黄酮进行快速的分离和纯化。

高速逆流色谱分离制备陈皮中的黄酮类化合物

应用高速逆流色谱法分离制备了陈皮中3种黄酮类化合物。以石油醚-乙酸乙酯-甲醇-水(体积比为2∶4∶3∶3)为两相溶剂系统,在主机转速850r/min、流动相流速1.7mL/min、检测波长280nm条件下进行分离制备,6h内从4.0g陈皮粗提物中一步分离制备得到橙皮苷10.1mg、桔皮素49.8mg和5-羟基-6,7,8,3′,4′-五甲氧基黄酮50.6mg,纯度均达97.0%以上,各化合物结构经质谱和核磁共振氢谱、碳谱鉴定。利用该方法可以对陈皮中的黄酮类化合物进行快速的分离和纯化。

高速逆流色谱分离纯化九里香中的黄酮类化合物

应用高速逆流色谱法分离纯化了九里香中的4种黄酮类化合物。以石油醚-乙酸乙酯-甲醇-水(5:5:4.8:5,v/v/v/v)作为两相溶剂系统,上相为固定相,下相为流动相,以主机转速800r/min、流速2.0mL/min、单次进样量200mg的条件成功地从4.0g九里香粗提物中分离纯化出54.31mg5,7,3′,4′,5′-五甲氧基黄酮(重结晶后)、107.68mg5-羟基-6,7,3′,4′-四甲氧基黄酮、215.54mg5-羟基-6,7,8,3′,4′-五甲氧基黄酮、84.36mg5-羟基-6,7,8,3′,4′,5′-六甲氧基黄酮,纯度均在95%以上。各化合物的结构均由质谱和核磁共振氢谱、碳谱鉴定。其中化合物5-羟基-6,7,3′,4′-四甲氧基黄酮为首次从九里香中分离得到。