模拟移动床色谱分离甘草苷和甘草素

以十八烷基硅烷键合硅胶(ODS)为固定相,V(乙醇)∶V(水)=30∶70为流动相的模拟移动床色谱(SMBC)体系对甘草黄酮中甘草苷与甘草素进行连续分离。SMBC体系设置洗脱带Ⅰ:1根色谱柱;精制带Ⅱ:2根色谱柱;吸附带Ⅲ:2根色谱柱,Ⅰ带独立,Ⅰ带洗脱液为乙醇。按照理想三角形理论选择SMBC操作参数,操作参数包括流动相流速、进料液流速和切换时间。结果表明:接近三角形底边选择SMBC的操作条件,在萃余液出口得到甘草苷,HPLC纯度高于70.44%,收率高于95.17%,同时在萃取液出口得到甘草素,HPLC纯度高于73.10%,收率高于90.74%,SMBC能有效分离甘草苷和甘草素。甘草苷萃余液和甘草素萃取液分别经浓缩、重结晶后,两种产品HPLC纯度均超过96%。     

填料粒径对制备色谱生产的影响

随着绿色精细化工工业的发展,对制备色谱和模拟移动床色谱(SMBC)的需求越来越大。填料粒径的选择是制备色谱和模拟移动床色谱分离中的关键问题。填料粒径主要从柱效和压力两方面影响着制备色谱的应用。压力影响着运行成本,柱效影响着分离效果,但两者又互相制约。该文利用板高曲线和压力变化曲线斜率积对填料性能进行了比较。斜率积消除了填料粒径的影响,却又联系着其他与柱压力和柱效相关的因素。利用斜率积来评价填料性能对问题的分析更加深入。该文通过对不同粒径填料所填充柱的孔隙率、柱压和柱效的比较发现,随填料粒径减小,柱压力的上升幅度小于随填料粒径平方反比例增大的幅度,理论塔板高度减小。从银杏黄酮的模拟移动床色谱分离结果可以看出,使用粒径为20~25μm的填料,其产品纯度低于使用粒径为30~40μm的填料。     

狭瓣鹰爪花枝叶中化学成分研究

综合运用硅胶柱色谱、反相硅胶柱色谱、Sephadex LH-20凝胶柱色谱以及制备型高效液相等色谱分离技术,对番荔枝科鹰爪花属植物狭瓣鹰爪花Artabotrys hainanensis枝叶中的化学成分进行系统研究。结合理化性质和多种现代波谱技术,并通过与文献进行对照,鉴定了从狭瓣鹰爪花枝叶90%乙醇提取物的中分离得到6个化合物,分别鉴定为:5-羟基-7,8-二甲氧基二氢黄酮(1)、litseachromolaevane A(2)、liguducin A(3)、1β-hydroxy-4(15),5E,10(14)-germacratriene(4)、(9E,11Z)14-hydroxyoctadecan-9,11-dienoic acid(5)和benzyl benzoate(6)。其中化合物1为黄酮类化合物,化合物2-4为倍半萜类化合物,化合物5为脂肪酸类化合物,化合物6为芳酸类化合物,所有化合物均为首次从鹰爪花属植物中分离得到。     

基于双部分丢弃的模拟移动床产率提高策略

在保证产品纯度的情况下,提出一种带额外色谱柱的双部分丢弃策略以提高模拟移动床的产率。通过将工艺点选取在纯提取产品和非纯提余产品区域以增大进料流量,并将由此导致的含较多杂质的提余产品暂时丢弃。丢弃的提余产品作为循环进料通入到一个额外色谱柱中以进一步分离,部分不能达到指定纯度的额外产品被永久丢弃。在模拟移动床和额外色谱柱处分别收集到的产品组成总产品。分析了工艺点的选取、提余产品的积分纯度阈值和额外产品的积分纯度阈值对总产品性能参数的影响。研究结果表明,所提策略能够以较高的回收率利用原料,且能够显著提高分离过程的产率,其分离效果优于传统的模拟移动床工艺和部分丢弃策略。     

基于双部分丢弃的模拟移动床产率提高策略

在保证产品纯度的情况下,提出一种带额外色谱柱的双部分丢弃策略以提高模拟移动床的产率。通过将工艺点选取在纯提取产品和非纯提余产品区域以增大进料流量,并将由此导致的含较多杂质的提余产品暂时丢弃。丢弃的提余产品作为循环进料通入到一个额外色谱柱中以进一步分离,部分不能达到指定纯度的额外产品被永久丢弃。在模拟移动床和额外色谱柱处分别收集到的产品组成总产品。分析了工艺点的选取、提余产品的积分纯度阈值和额外产品的积分纯度阈值对总产品性能参数的影响。研究结果表明,所提策略能够以较高的回收率利用原料,且能够显著提高分离过程的产率,其分离效果优于传统的模拟移动床工艺和部分丢弃策略。     

高效液相色谱法分离纯化酯型儿茶素的研究

采用反相高效液相色谱技术 ,分离制备粗儿茶素粉末中表没食子儿茶素没食子酸酯( EGCG)、没食子儿茶素没食子酸酯 ( GCG)、表儿茶素没食子酸酯 ( ECG)三种酯型儿茶素馏分。制备色谱条件 :色谱柱 ,( 80 mm i.d× 5 0 0 mm,Fuji C18,粒径 2 5～ 40 μm) ;流动相 :有机醇 A- 1 /水( 1 6.5 /83.5 ,v/v,流速为 5 8m L/min;检测波长 2 78nm,进样量 30 0 0 mg。将所收集相应馏分分别经 P- 1大孔树脂吸附脱去溶剂 ,低沸点溶剂洗脱 ,旋转蒸发浓缩洗脱液 ,冷冻干燥后 ,得到 EGCG、GCG、ECG白色粉末。各物质经 HPLC检测纯度达 99.2 %以上。该法适用于分离纯化 EGCG、GCG、ECG三种酯型儿茶素单体     

《室内装饰装修材料 胶粘剂中有害物质限量》国家标准简介(下)

3 .3　胶粘剂中甲苯、二甲苯含量的测定3.3.1　测定方法试样用适当的溶剂稀释后 ,直接用微量注射器将稀释后的试样溶液注入进样装置 ,并被载气带入色谱柱 ,在色谱柱内被分离成相应的组分 ,用氢火焰离子化检测器检测并记录色谱图 ,用外标法计算试样溶液中甲苯和二甲苯的含量。3.3.2　测定条件1 .汽化室温度 :2 0 0℃ ;2 .检测室温度 :2 5 0℃ ;3.检测器 :氢火焰离子化检测器 ;4.色谱柱 :毛细管柱 (ＤＢ 1 :固定液为二甲基聚硅氧烷 ,30ｍ× 0 .5 3ｍｍ× 1 .5 μｍ) ;5 .载气 :氮气 ,纯度大于 99.9% ,其柱前压为 70ｋＰａ( 35℃ ) ;6.程序升温…     

异叶三宝木中倍半萜类化学成分研究

综合运用硅胶柱色谱、ODS反相硅胶柱色谱、Sephadex LH-20凝胶柱色谱及制备型高效液相等现在色谱分离技术对大戟科三宝木属植物异叶三宝木Trigonostemon heterophyllus枝叶中的化学成分进行系统的分离和纯化。根据化合物的理化性质和波谱数据,并通过与文献对照,鉴定了从异叶三宝木枝叶85%乙醇提取物的石油醚萃取部位中分离得到的8个倍半萜类化合物,分别鉴定为:9-hydroxy-4,7-megastigmadien-3-one(1)、9,10-dihydroxy-4,7-megastigmadien-3-one(2)、blumenol A(3)、4,5-dihydroblumenol A(4)、dehydrovomifoliol(5)、3-hydroxy-β-ionone(6)、sarmentol F(7)和5,12-epoxy-9-hydroxy-7-megastigmen-3-one(8)。所有化合物均为首次从三宝木属植物中分离得到。     

负载Ag~+ D72树脂色谱柱分离纯化花生四烯酸工艺的建立

目的建立负载Ag+D72树脂色谱柱分离纯化花生四烯酸(Arachidonic acid,AA或ARA)的工艺。方法采用负载Ag+D72树脂色谱柱对微生物油脂中的ARA进行分离纯化,确定最佳分离纯化参数,利用气相色谱法检测ARA的含量。结果负载Ag+D72树脂的最大饱和吸附量约为9 mg/g干树脂,在吸附温度0℃、不饱和脂肪酸甲酯上样质量浓度5 mg/ml,5%丙酮正己烷溶液(体积比)洗脱、解吸温度30℃、洗脱流速2 ml/min的条件下,ARA的纯度达89.4%,收率达79.3%。结论负载Ag+D72树脂色谱柱可有效分离纯化微生物油脂中的ARA,为进一步生产高纯度的ARA,进而规模化生产ARA产品提供了参考。     

茄尼醇的SFC制备色谱分离工艺

采用ZORBAX SB-C18(250 mm×9.4 mm I.D.,5 μm)色谱柱为固定相,SC-CO2/甲醇为流动相,考察了超临界流体色谱分离提纯烟草萃取物中茄尼醇的工艺条件、流动相流速和改性剂含量对分离度的影响,以及温度和压力对茄尼醇容量因子、茄尼醇与相邻色谱峰组分分离度和选择性因子的影响.通过采用选定SFC分离工艺条件,茄尼醇产品纯度达到94.9%.     

模拟移动床色谱拆分奥美拉唑对映体

以乙醇为流动相,用纤维素三苯基氨基甲酸酯涂敷型手性固定相在模拟移动床色谱上拆分了奥美拉唑对映体.研究了柱子切换时间以及流动相内部流速对分离效果的影响.实验条件下,S-奥美拉唑的浓度、产率和回收率随切换时间增加而增加,流动相消耗和纯度则随之降低.降低内部流速,有利于改善分离,S-奥美拉唑的纯度最高可达96.4%,R-奥美拉唑的纯度最高为88.4%.     

人参皂甙Rb_1的模拟移动床分离

介绍了应用模拟移动床技术分离高含量人参皂甙Rb1的工艺。确定了模拟移动床分离人参皂甙Rb1的操作条件,洗脱剂:V(甲醇)∶V(水)=45∶55;模式:1-4-3;切换时间:360 s;洗脱流速:60 mL/min;萃取液流速:30mL/min;进样流速:3 mL/min;样品质量浓度:0.2 g/mL。讨论了影响模拟移动床分离的主要因素,并与单柱分离工艺进行了比较。     

高速逆流色谱快速分离四种甘草黄酮及其结构鉴定

通过高速逆流色谱从新疆产甘草粗提物中分离得到甘草黄酮醇、甘草素、芒柄花素和甘草异黄酮甲四种甘草类黄酮。溶剂系统为正己烷-乙酸乙酯-甲醇-水（1：2：1：1）,上相作为固定相,下相作为流动相,主机旋转方向为顺时针,转速850rpm,流速4．0mL／min,检测波长260nm。经过160min分离,从400mg甘草粗提物中得到甘草黄酮醇26mg、甘草素8mg、芒柄花素12mg、甘草异黄酮甲10mg,纯度分别为96．3％、95．7％、98．5％、98．8％。结构经熔点、UV、MS、^1H—NMR和^13C-NMR鉴定。     

Separation of Close-Boiling Components Using a New Chromatographic Method

Abstract

A combined continuous and preparative system of gas-liquid chromatography was developed and used for the separation of the close-boiling components diethyl ether and dichloromethane. In this system the less-absorbed component in the mixture can be obtained continuously in an almost pure state in one section and the remaining components can be separated in the other section of the column. Several experimental conditions (e.g., column length, particle size, feed concentration, and flow rates of carrier gas and desorbent) were varied in order to evaluate their effects on the performance of the chromatographic system. From the results of the experiments, additional column length and desorbent velocity were found to be the most important factors in separating the feed mixture continuously. The optimum switching time for good separation was experimentally measured, and it was mainly affected by column temperature and column length if the feed mixture and stationary phase were fixed. Throughputs of between 5 to 10 cm³/h resulted in good purity under certain experimental conditions.     

模拟移动床色谱手性分离过程的非线性非理想模型

A non-linear non-ideal model,taking into account non-linear competitive isotherms,axial disperison,film mass transfer,intraparticle diffusion,and port periodic switching,was developed to simulate the dynamics of simulated moving bed chromatography(SMBC),The model equations were solved by a new efficient numerical technique of orthogonal collocation on finite elements with periodical movement of conceantration vector,The simulated SMBC performance is in accordance with the experimental results reported in the literature for separation of 1,1‘‘‘‘‘‘‘‘-bi-2-naphtol enantiomers using SMBC,This model is useful for design,operation ,optimization and scale-up of non-linear SMBC for chiral separations with significant non-ideal effects,especially for high solute concentration and small intraparticle diffusion coefficient or large chiral stationary phase particle.     

One Step Large-Scale Separation and Purification of Rutin from Boenninghausenia sessilicarpa by Countercurrent Chromatography

In this study, a preparative countercurrent chromatography (CCC) method for isolation and purification of the bioactive component rutin directly from the ethanol extract of Boenninghausenia sessilicarpa was successfully established by using n-butanol-ethyl acetate-water as the two-phase solvent system. The upper phase of n-butanol-ethyl acetate-water (4:1:5, v/v) was used as the stationary phase of CCC. Under the optimum conditions, 112 mg of rutin at 98.6% purity was obtained from 2.0 g of the crude extract in a single CCC separation. The peak fraction of CCC was identified by negative ESI, ¹H NMR, and ¹³C NMR.     

Two-step chromatographic procedure for the preparative separation and purification of epigallocatechin gallate from green tea extracts

The preparative separation and purification of epigallocatechin gallate (EGCG) from green tea extracts was achieved by a two-step chromatographic procedure. In the first step, a preparative β-cyclodextrin (β-CD) bonded silica chromatography operated in the polar organic mode using methanol/acetonitrile/acetic acid as the mobile phase was applied. Due to a high selectivity for EGCG over epicatechin (EC) and caffeine (CA), an efficient separation of EGCG from EC and CA was achieved and the system could be scaled-up with high recovery of EGCG (>90%). The EGCG-rich fraction obtained from the first step was subjected to the second step where a preparative C-18 chromatography operated in the reversed-phase mode using water/methanol/acetic acid as the mobile phase was applied. The resolution of EGCG was significantly enhanced as the sample contained no EC and CA. The system could also be scaled-up and both the purity and recovery of EGCG reached about 90%. In summary, the chromatographic procedure consisting of two such complementary steps gave a satisfactory purification results: the purity and recovery of EGCG were >90% and >80%, respectively. Most significantly, the purification method could be more easily scaled-up, showing good potential for industrial applications.     

超临界流体色谱法制备高纯度EPA-EE和DHA-EE

以二氧化碳作流动相,分别以极性相反的C18柱和硅胶柱为固定相,用超临界流体色谱法分离二十碳五烯酸乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE)。比较C18柱和硅胶柱分离EPA-EE和DHA-EE的机理和分离效果,提出结合C18柱和硅胶柱的超临界流体色谱制备高纯度EPA-EE和DHA-EE的方法。     

One Step Purification of Piperine Directly from Piper nigrum L. by High Performance Centrifugal Partition Chromatography

Abstract

In this study, a preparative high performance centrifugal partition chromatography (HPCPC) method for isolation and purification of the bioactive component piperine directly from the ethanol extract of Piper nigrum L. was successfully established by using n-hexane-ethyl acetate-methanol-water as the two-phase solvent system. The upper phase of n-hexane-ethyl acetate-methanol-water (6:5:6:5, v/v) was used as the stationary phase of CPC. Under the optimum conditions, 40 mg of piperine at 98.5% purity, as determined by HPLC, was yielded from 300 mg of the crude extract in a single CPC separation. The peak fraction of CPC was identified by ¹H NMR and ¹³C NMR.