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在现代分离科学中,手性化合物的分离分析一直是研究的重点和难点。相比于高效液相色谱(HPLC)、气相色谱(GC)等传统色谱分析方法,毛细管电泳(CE)技术凭借其高效率、低消耗、分离模式多样化等诸多优势,已经发展成为手性分离研究领域最有应用前景的分析方法之一。近年来,研究人员在CE手性分析方法的构建过程中,基于毛细管电动色谱(EKC)、配体交换毛细管电泳(LECE)、毛细管电色谱(CEC)等各种基础电泳模式,不断地对传统手性分离体系进行优化和改造,构建出了许多高性能的新型手性CE分离体系。如利用各类功能化离子液体以"手性离子液体协同拆分""手性离子液体配体交换""离子液体手性选择剂"等模式设计出多种基于离子液体的CE手性分离体系;利用纳米材料独特的尺寸效应、多样性、可设计性等特点,直接或与传统手性选择剂有机结合构建CE手性分离体系。此外,金属有机骨架材料修饰、低共熔溶剂修饰、非连续分段式部分填充等各式新颖的CE手性分离体系也都被研究人员成功开发,并表现出较大的发展潜力。该综述将对近年来(尤其是2015~2019年)此类新型CE手性分离体系的发展状况进行梳理,并结合相应的手性识别机理研究和手性CE方法实际应用情况,对该领域存在的问题及发展前景进行分析和展望。 相似文献
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总结了手性逆流色谱的5个特点,系统地介绍了逆流色谱的手性分离以及高速逆流色谱手性分离中氨基酸衍生物、环糊精衍生物、手性有机酸、多糖衍生物、牛血清白蛋白等手性选择剂的应用。 相似文献
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手性固定相-高效液相色谱法在手性药物、手性农药等的分离分析中应用广泛。本文采用3种多糖衍生物的手性固定相(即EnantioPak AD、AS和OD)对20种手性化合物开展手性分离研究,进而探讨样品分子结构、多糖骨架和衍生基团对手性分离的影响。结果表明,除化合物13外,其余化合物在EnantioPak AD上均实现基线分离,分离度多在2.0以上,在正己烷-醇流动相中加入酸碱添加剂可改善和优化酸性或碱性化合物的分离效果;芳香醇(化合物13~16)随着侧链碳数增加在色谱柱上的保留减弱,其分离度呈现增加的趋势;对比8种化合物在3种手性固定相上的分离结果可知,EnantioPak AD表现出更优的分离性能。这为深入研究和了解多糖手性固定相、拓展其手性分离应用提供了参考。 相似文献
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卡替诺尔和氟西汀对映体的高效毛细管电泳分离 总被引:2,自引:2,他引:0
考察了以羧甲基-β-(环糊精-β-CD)、β-环糊清(β-CD)、羟丙基-β-环糊精(HP-β-CD)、二甲基-β-环糊精(DM-β-CD)为手性选择剂,在50mmol/L醋酸三乙胺缓冲溶液中分离卡替诺尔和氟西汀对映体。该文还通过考察手性选择剂的浓度、背景电解质的酸度、背景电解质的类型等因素对映体手性分离的影响,对分离条件进行了优化,初步探讨了手性识别机理。实验结果表明:用约4mmol/L的CM-β-CD分离氟西汀和卡替诺尔对映体,能使对映体达到良好分离,不仅节约了分析成本,也简化了分析过程。 相似文献
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双动态吸附毛细管电色谱的手性分离——采用阳离子表面活性剂和阴离子手性选择剂作为假固定相 总被引:2,自引:2,他引:0
建立了以十六烷基三甲基溴化铵或1,5-二甲基-1,5-二氮杂十一烷亚甲基聚N-甲溴化物为阳离子表面活性剂,并以磺丁基β-环糊精为手性选择剂的双动态吸附毛细管电色谱。以碱性的丙比胺和酸性的华法林作为拆分对象,考察了双动态吸附毛细管电色谱的手性分离行为,以及动态吸附柱的重复性。在双动态吸附毛细管电色谱条件下,丙比胺和华法林的手性分离度较大,丙比胺的分离度可达3.21,丙比胺连续进样10次,迁移时间的相对标准偏差小于1.0%。 相似文献
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A rapid and effective method was developed for the chiral separation of raltitrexed (RD) enantiomers by carboxymethyl-beta-cyclodextrin
(CM-β-CD)-modified micellar electrokinetic chromatography (MEKC). Optimization of conditions including the type and concentration
of the chiral selector, concentration of sodium dodecyl sulfate (SDS), pH and concentration of the background electrolyte
(BGE), capillary temperature, and applied voltage was investigated. The enantiomers of raltitrexed could be separated with
satisfactory resolution and linear response by using 75 mM Tris-phosphate at pH 8.0 containing 30 mM SDS and 8 mM CM-β-CD
as buffer system. Furthermore, the usefulness of this method was demonstrated in a purity test of a real synthetic drug sample.
Figure Chiral separation of raltitrexed by CM-β-CD MEKC was optimized and applied to test the purity of a synthetic drug sample 相似文献
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Magdalena C. Waldhier Michael A. Gruber Katja Dettmer Peter J. Oefner 《Analytical and bioanalytical chemistry》2009,394(3):695-706
Free amino acids are typically quantified as the sum of their enantiomers, because in terrestrial organisms they mainly exist
in the left-handed form. However, with increasing understanding of the biological significance of right-handed amino acids
interest in enantioselective quantification of amino acids has steadily increased. Initially, electrophoretic and chromatographic
methods using chiral (pseudo)-stationary phases or chiral eluents were applied to the separation of amino acid enantiomers.
Later, derivatization of amino acids prior to chromatography with chiral reagents gained in popularity, because the diastereomers
formed can be resolved on conventional reversed-phase columns. Novel multi-interaction chiral columns turned attention back
to direct chiral chromatographic methods. Hyphenation to mass spectrometry has increasingly replaced optical detection because
of superior selectivity, although this has not obviated the need for baseline resolution of amino acid enantiomers. Despite
the progress made, enantioselective separation and quantification of amino acids remains an analytical challenge owing to
frequently incomplete resolution of all naturally occurring enantiomers and insufficient sensitivity for the determination
of the trace amounts of d-amino acids typically found in biological fluids and tissues.
Chiral GC-MS analysis of heptafluorobutanol/pentafluoropropionanhydride amino acid derivatives on an Rt-gDEXsa column 相似文献
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Han X Wang C He L Beesley TE Armstrong DW 《Analytical and bioanalytical chemistry》2007,387(8):2681-2697
A new synthetic polymeric chiral stationary phase for liquid chromatography was prepared via free-radical-initiated polymerization
of trans-9,10-dihydro-9,10-ethanoanthracene-(11S,12S)-11,12-dicarboxylic acid bis-4-vinylphenylamide. The new polymeric chiral stationary phase (CSP) showed enantioselectivity
for many chiral compounds in multiple mobile phases. High stability and sample capacities were observed on this polymeric
chiral stationary phase. Mobile phase components and additives affected chiral separation greatly. This new synthetic chiral
stationary phase is complementary to two other related commercially available CSPs: the P-CAP and P-CAP-DP columns. Interactions
between the chiral stationary phase and analytes that lead to retention and chiral recognition include hydrogen bonding, dipolar,
and π–π interactions. Repulsive (steric) interactions also contribute to chiral recognition.
Figure LC chromatograms showing the analytical (blue) and preparative (red) separations of N-(3,5-dinitrobenzoylleucine) enantiomers on a new synthetic polymeric chiral stationary phase 相似文献
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Christian V. Hoffmann Michael Lämmerhofer Wolfgang Lindner 《Analytical and bioanalytical chemistry》2009,393(4):1257-1265
A recently reported chiral strong cation exchanger (cSCX) type stationary phase was investigated for the LC separation of
a series of Cinchona alkaloids and synthetic derivatives thereof to test its usefulness as alternative methodology for the separation of those
important pharmaceuticals. The cSCX column-packing material was qualitatively compared on the one hand against a commercially
available non-enantioselective SCX-material, PolySulfoethyl-A, and, on the other hand, against a modern C18 reversed-phase
stationary phase which is commonly employed for Cinchona alkaloid analysis. Both SCX columns showed no pronounced peak-tailing phenomena which typically hamper Cinchona alkaloid RP analysis and require specific optimization. Thus, the cSCX-based assay provided new feasibilities for the separation
of the Cinchona alkaloids in polar organic mode as opposed to conventional reversed-phase methodologies. In particular, a method for the
simultaneous determination of eight Cinchona alkaloids (quinine, quinidine, cinchonine, cinchonidine, and their corresponding dihydro analogs) using the cSCX column in
HPLC has been developed and exemplarily applied to impurity profiling of a commercial alkaloid sample. Furthermore, both SCX
materials allowed successful separation of C9-epi and 10,11-didehydro derivatives from their respective educts in an application
in synthetic Cinchona alkaloid chemistry.
Figure An alternative separation principle - HPLC separation of strongly basic natural Cinchona alkaloids and synthetic derivatives thereof by means of a strong cation-exchanger type chiral stationary phase 相似文献