烯丙基乙基醚接枝聚硅氧烷气相色谱固定相的研究

合成了侧链为烯丙基乙基醚的聚硅氧烷气相色谱固定相,静态法涂柱,评价了其色谱性能.该固定相柱效高,易于涂渍,耐温达290℃,分离选择性好,适用于醇类和酯类的分离以及白酒样品的分析.     

气相色谱手性固定相研究进展

本文评述了气相色谱手性分离的发展过程,介绍了氨基酸、二肽、金属配合物、环糊精、多糖、手性离子液体、环肽、键合以及交联类气相色谱手性固定相以及各类型的拆分机理,展望了气相色谱手性固定相的研究前景。     

气相色谱手性固定相研究进展

本文评述了气相色谱手性分离的发展过程,介绍了氨基酸、二肽、金属配合物、环糊精、多糖、手性离子液体、环肽、键合以及交联类气相色谱手性固定相以及各类型的拆分机理,展望了气相色谱手性固定相的研究前景.     

Polysiloxane with Pendant [60]Fulleropyrrolidines as Stationary Phase for Capillary Gas Chromatography

Fullerenesciencehasdevelopedquiterapidlysincethediscoveryofthebulkpreparationmethodoffullerenesinl99o.Duetotherichnessofunusualstructuresandoutstandin2thepreparationofaHPLCmicrocolumn,whichwasshowntobeabletoseparatCamixtureofCooandC7oandalsoamixtureofcalixarenesl.AfulleropyrrolidinederivativewhichisattachedcovalentlytosilicagelinHPLCshowedmolecularrecognitiontowardscalixarenes,cyclodextrinsandsomehelical-shapedpeptides'.Surface-linkedCoc7o-polystyrenedivinylbenzenebeadsasachromatographicm…     

新型多孔材料用作色谱手性固定相

手性固定相是色谱法分离分析手性化合物的关键。近年来,随着材料科学的迅速发展,越来越多的新型手性材料被作为色谱固定相用于手性分离分析。本文综述了近5年来液相色谱、气相色谱和毛细管电色谱领域的新型手性固定相的研究进展,重点总结了基于手性多孔材料的新型手性固定相研究,最后对手性固定相的研究进行了总结与展望。     

C_(60)侧链线性聚硅氧烷毛细管气相色谱固定相的制备与色谱性能

首次以含氢硅油依次与溴丙烯、叠氮钠及Ｃ６０反应合成了两种新的Ｃ６０侧链线性聚硅氧烷并用作毛细管气相色谱固定相。该类固定相柱效高,使用温度范围宽,热稳定性好,最高柱温达３６０℃,基线漂移量为３０～４０ｆＡ,呈弱极性,对各种醇、酮、芳胺、多环芳烃、邻苯二甲酸酯类有良好的分离选择性,尤其对各类位置异构体有着独特的分离效果。     

2,3-Di-O-pentyl-6-O-tert-butyldimethylsilyl-β-cyclodextrin as a Chiral Stationary Phase in Capillary Gas Chromatography

2,3-Di-O-pentyl-6-O-tert-butyldimethylsilyl-β-cyclodextrin has been evaluated as an enantioselective stationary phase for capillary gas chromatography. Experimental results show a good enantioselectivity towards compounds with different functional groups (haloalkanes, alcohols, esters, terpenoids, amino acid derivatives, and heterocycles). Column stability improves mixing the chiral phase with polysiloxane SE-54 (1 : 1).     

新型侧链聚硅氧烷高分子液晶作毛细管柱气相色谱固定液的研究

 以合成的新型胆甾酯类侧链聚硅氧烷高分子液晶作固定液 ,涂渍在弹性石英毛细管柱上 ,获得了具有较高的柱效和选择性、良好的热稳定性、适于分离多种异构体混合物的毛细管柱。     

新型高效液相手性固定相选择剂——大环抗生素

 综述了大环抗生素类手性固定相在高效液相中的应用和最新发展动态,根据其分子结构探讨了其手性分离的特点,并与其他类型的手性固定相进行了比较;共51篇。     

双活性官能团冠醚固定相的合成及毛细管柱的研制

本项研究合成了一种新的气相色谱固定相：３－端烯丙基－不对称二苯并１４－冠－４－二羟基冠醚。其结构经元素分析、红外光谱、核磁共振及质谱的数据证实。将这种固定相涂渍在弹性石英毛细管内,测定其柱效、热稳定性、平均极性及选择性。结果表明：该固定相具有良好的色谱特性,对某些极性位置异构体有着良好的选择性。     

Cellulose Derivatives Used as Chiral Stationary Phases in Capillary Gas Chromatography

Abstract

In this work, we present the first separation of enantiomers in gas chromatography (GC) using a fused‐silica capillary column containing cellulose triacetate, cellulose triphenylcarbamate, or cellulose tris(3,5‐dimethylphenylcarbamate) as the new chiral stationary phase. The separated solutes included alcohols, amine, ketone, ether, ester, and amino acid. Their column efficiency, polarity, and chiral selectivity were studied. The retention mechanism was discussed. The results showed that those derivatives had relatively high chiral recognition abilities and can be used as the chiral stationary phases in GC.     

缬氨霉素作为毛细管气相色谱新型固定相的性能研究

本文研究了缬氨霉素的气相色谱特性, 考察了它们对一些难分离物质对、位置异构体以及一些手性化合物的分离效果. 除文献[3]外, 目前尚未见到有关将环状肽作为色谱固定相的报道.     

环糊精衍生物气相色谱手性毛细管柱的制备与考察

合成了３种新的含长烷基链的β－环糊精衍生物手性固定相。实验表明，随着烷基链长的增加，对手性卤代烃和酯的立体选择性有所提高；以ＯＶ－７为手性固定相的稀释剂对多数手性化合物的拆分效果好于ＯＶ－１７０１。２，６－Ｏ－二辛基－３－Ｏ三氟乙酰－β－环糊精／ＯＶ－７柱应用于不对称合成及催化中对映体的分离与测定和白酒中乳酸乙酯对映体含量的测定。     

异喹啉酸衍生物配体交换色谱手性固定相的制备及应用

合成了2-(2-羟基十六烷基)-(S)-1,2,3,4-四氢-3-异喹啉羧酸手性选择子,并采用动态涂渍方法,制备了一种涂渍于ODS柱上的新型手性配体交换色谱固定相。采用醋酸铜水溶液为流动相,在柱温25℃和UV254nm检测条件下,拆分了16种D,L-氨基酸对映体,其对映体选择性α和分离度Rs分别在1.09~1.67和1.0~4.8之间,并观察到D-异构体在先,L-异构体在后的色谱流出顺序。讨论了柱温、流动相的流速、pH值、Cu2 浓度和NH4 对D,L-氨基酸对映体拆分的影响。     

纤维素衍生物作为毛细管气相色谱新型固定相的研究

以纤维素三苯甲酸酯、纤维素三苯基氨基甲酸酯以及二者的混合物为固定相,制备了新型毛细管气相色谱柱,最高柱效达到2580板/米。其能对一些难分离物质对、位置异构体以及手性化合物进行拆分,如对丙氨酸的分离因子可达到1·13。此外,还研究了毛细管柱的极性、选择性以及保留机理。结果表明,该类聚合物是一类很有前景的新型气相色谱固定相。     

Design,Preparation and Application of a New π‐Basic Chiral Stationary Phase for the Liquid Chromatographic Separation of Enantiomers

A new reciprocal π‐basic chiral stationary phase (CSP) was designed based on the reciprocity conception of chiral recognition and prepared starting from (S)‐leucine. The CSP thus prepared was applied in resolving various π‐acidic N‐(3,5‐dinitrobenzoyl)‐α‐amino amides and esters and found to be very effective. Especially, N‐(3,5‐dinitrobenzoyl)‐α‐amino N,N‐dialkyl amides were resolved very well on the new reciprocal CSP. From the chromatographic resolution results and based on the reciprocity conception of chiral recognition with the aid of Corey/Pauling/Koltan (CPK) molecular model studies, a chiral recognition mechanism which utilizes π‐π interaction and simultaneously two hydrogen bonding interactions between the CSP and the analyte has been proposed. The CSP prepared in this study was also successful in resolving 3,5‐dinitrophenylcarbamate derivatives of 2‐hydroxycarboxylic acid esters.     

高效液相色谱蛋白质手性固定相

本文综述了近年文献中已报道的各种高效液相色谱蛋白质（酶）手性固定相及其在手性拆分中的应用，并阐述了蛋白质作为手性选择剂拆分机理的研究进展。     

A Chiral Recognition Mechanism Proposed for Resolving π-Acidic Racemates on π-Acidic Chiral Stationary Phases Derived from (S)-Leucine

A chiral recognition mechanism which can rationalize the resolution of N-(3,5-dinitrobenzoyl)-α-amino amides on chiral stationary phases (CSPs) obtained from N-(3,5-dinitrobenzoyl)leucine amide derivatives has been proposed on the basis of the chromatographic resolution behavior of various N-(3,5-dinitrobenzoyl)-α-amino acid derivatives and N-(various benzoyl)leucine N-propyl amides. The proposed chiral recognition mechanism utilizes two hydrogen bonding interactions between the CSP and the analyte and a π-π donor-acceptor interaction between the N-(3,5-dinitrobenzoyl) groups of the CSP and the analyte. From the chiral recognition mechanism proposed, it has been concluded that the resolution of π-acidic N-(3,5-dinitrobenzoyl)-α-amino acid derivatives on π-acidic CSPs derived from N-(3,5-dinitrobenzoyl)leucine amide delivatives is not unusual, but is merely the extension of the resolution of the π-basic racemates on π-acidic CSPs. However, the chromatographic behavior of the resolution of N-(3,5-dinitrobenzoyl)phenylglycine derivatives on CSPs derived from N-(3,5-dinitrobenzoyl)leucine amide derivatives is different from that of the resolution of other N-(3,5-dinitrobenzoyl)-α-amino acid derivatives. To rationalize this exceptional behavior, a second chiral recognition mechanism which utilizes two hydrogen bonding interactions (which are different from those of the first chiral recognition mechanism) between the CSP and the analytes and a π-π donor-acceptor interaction between the N-(3,5-dinitrobenzoyl) group of the CSP and the phenyl group of the analytes has been proposed to compete with the first chiral recognition mechanism. In this instance, it has been proposed that the separation factors and the elution orders of the resolution of N-(3,5-dinitrobenzoyl)phenylglycine derivatives are dependent on the balance of the two competing chiral recognition mechanisms.     

高效液相色谱手性固定相法拆分克伦特罗对映体

以正己烷、异丙醇为流动相,用Whelk-O1手性固定相成功拆分了药物克伦特罗对映体。出峰时间在5min左右,峰形对称性好,完全达到基线分离,分离因子大于1．4,可用于该对映体药物的分析与制备分离。讨论了二元流动相中异丙醇含量及温度的变化对分离的影响,并对拆分机理进行了探讨。