共查询到19条相似文献,搜索用时 93 毫秒
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本文建立了一种快速、简单拆分手性药物"罗格列酮"的新方法。采用本实验室合成的天冬氨酸-β-环糊精为手性选择剂,在毛细管区带电泳中对罗格列酮进行拆分,通过优化影响实验的主要因素(手性选择剂浓度、缓冲溶液pH、柱温及分离电压),得到了使罗格列酮达到基线分离的最佳实验条件。 相似文献
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采用非手性的Cu色谱柱,通过在流动相中加入手性选择剂β-环糊精和在样品中加入β-环糊精的方法实现对盐酸西布曲明对映体的拆分.流动相组成为含β-环糊精的甲醇-水(50∶50,V/V,pH=6).当手性选择剂β-环糊精的浓度为0.8mmol/L时,盐酸西布曲明对映体在进样后的5.7min得到了基线分离. 相似文献
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Runqiang Liu Yijun Zhang Lianyang Bai Mingxian Huang Jun Chen Yuping Zhang 《International journal of molecular sciences》2014,15(4):6161-6168
A chiral selector of cellulose-2,3-bis(3,5-dimethylphenylcarbamate) (CBDMPC) was synthesized by reacting 3,5-dimethylphenyl isocyanate with microcrystalline cellulose dissolved in an ionic liquid of 1-allyl-3-methyl-imidazolium chloride (AMIMCl). The obtained chiral selector was effectively characterized by infrared spectroscopy, elemental analysis and 1H NMR. The selector was reacted with 3-aminopropylsilanized silica gel and the CBDMPC bonded chiral stationary phase (CSP) was obtained. Chromatographic evaluation of the prepared CSPs was conducted by high performance liquid chromatographic (HPLC) and baseline separation of three typical fungicides including hexaconazole, metalaxyl and myclobutanil was achieved using n-hexane/isopropanol as the mobile phase with a flow rate 1.0 mL/min. Experimental results also showed that AMIMCl could be recycled easily and reused in the preparation of CSPs as an effective reaction media. 相似文献
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A recycle HPLC system equipped with a polysaccharide‐based chiral column was used for the enantiomeric separation of asymmetric triacylglycerols (TAGs). When the chiral columns were screened by the resolution of 1,2‐dipalmitoyl‐3‐oleoyl‐rac‐glycerol separation was achieved only with the cellulose tris‐ (3,5‐dimethylphenylcarbamate) chiral selector. The resolution of other TAG enantiomers was also examined, and 1,2‐dioleoyl‐3‐palmitoyl‐rac‐glycerol, 1,2‐dipalmitoyl‐3‐linoleoyl‐rac‐glycerol, 1,2‐dipalmitoyl‐3‐eicosapentaenoyl‐rac‐glycerol, 1,2‐dipalmitoyl‐3‐docosahexaenoyl‐rac‐glycerol, and 1,2‐docosahexaenoyl‐3‐palmitoyl‐rac‐glycerol were resolved into their respective enantiomers. However, neither 1,2‐dioleoyl‐3‐linoleoyl‐rac‐glycerol, consisting of only unsaturated fatty acids, nor 1,2‐dipalmitoyl‐3‐stearoyl‐rac‐glycerol, consisting of only saturated fatty acids, was resolved. In addition, 1,2‐eicosapentaenoyl‐3‐palmitoyl‐rac‐glycerol was not resolved clearly, even in the recycle runs. These results suggest that asymmetric TAGs having both a palmitic acid moiety and an unsaturated fatty acid moiety at the sn‐1 or sn‐3 positions might be resolved on a cellulose tris‐ (3,5‐dimethylphenylcarbamate) chiral column. 相似文献
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Thomas Munkelt Christian Küster Dr. Christof Hamel Prof. Dirk Enke Prof. Andreas Seidel‐Morgenstern Prof. Andreas Seidel‐Morgenstern 《化学,工程师,技术》2013,85(11):1686-1693
Porous glass can be widely applied due to favorable chemical and physical properties and the possibility to modify the surface. This work describes the synthesis and optimization of porous glass beads for recovering chiral anesthetics and the separation of the enantiomers. Besides a characterization by nitrogen adsorption and mercury intrusion, the retention behavior of desflurane is investigated in chromatographic experiments with the native support and after immobilization of a chiral selector. 相似文献
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以7-CD为毛细管电泳手性选择剂,对苯氧羧酸类除草剂对映体的分离进行了研究。考察了手性选择剂的种类、7-CD浓度、SDS浓度、背景电解质浓度、pH值等对分离的影响。结果发现,选择30mmol·L11rCD+100mmol·L11SDS+75mmol·L-1H3P04作为电泳缓冲体系(pH值2.O),2,4-滴丙酸、2,4,5-滴丙酸、2-(3-氯苯氧基)丙酸对映体完全分离,2-(4-氯苯氧基)丙酸、2-苯氧基丙酸对映体部分分离,分离度分别为3.42、8.27、2.83、0.89、0.50。 相似文献
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Roberta Franzini Marco Pierini Andrea Mazzanti Antonia Iazzetti Alessia Ciogli Claudio Villani 《International journal of molecular sciences》2021,22(1)
The presence of stereogenic elements is a common feature in pharmaceutical compounds, and affording optically pure stereoisomers is a frequent issue in drug design. In this context, the study of the chiral molecular recognition mechanism fundamentally supports the understanding and optimization of chromatographic separations with chiral stationary phases. We investigated, with molecular docking, the interactions between the chiral HPLC selector Whelk-O1 and the stereoisomers of two bioactive compounds, the antiviral Nevirapine and the anticonvulsant Oxcarbazepine, both characterized by two stereolabile conformational enantiomers. The presence of fast-exchange enantiomers and the rate of the interconversion process were studied using low temperature enantioselective HPLC and VT-NMR with Whelk-O1 applied as chiral solvating agent. The values of the energetic barriers of interconversion indicate, for the single enantiomers of both compounds, half-lives sufficiently long enough to allow their separation only at critically sub-ambient temperatures. The chiral selector Whelk-O1 performed as a strongly selective discriminating agent both when applied as a chiral stationary phase (CSP) in HPLC and as CSA in NMR spectroscopy. 相似文献
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The distribution behavior of mandelic acid (MA) enantiomers was examined in a two‐phase system containing di(2‐ethylhexyl) phosphoric acid (D2EHPA) with two tartaric acid derivatives as complex chiral selectors in n‐octanol. Factors affecting the extraction were investigated, including the structure and concentration of tartaric acid as well as the concentration of D2EHPA and D,L‐MA. The results showed that both the distribution ratio and enantioselectivity were greatly improved by using a complex chiral selector rather than using the tartaric acid derivative by itself. Finally, it was found that the formation of mixed complex chiral selectors by mixing two tartaric acid derivatives with D2EHPA can improve the capacity of enantioselective extraction. 相似文献