共查询到19条相似文献,搜索用时 140 毫秒
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以2,4-二硝基氟苯为衍生化试剂,建立柱前衍生化结合手性固定相高效液相色谱法拆分2-甲基哌嗪对映体的方法。采用Chiralpak IA(250 mm×4.6 mm,5μm)手性色谱柱,流动相为V(正己烷)∶V(无水乙醇)∶V(二乙胺)=50∶50∶0.1,检测波长261 nm,流速0.5 mL/min,柱温30℃。在此优化试验条件下,衍生后的对映体分离度达3以上,在0.15~1.5μg/mL浓度范围内线性关系良好,连续重复进样6次,相对标准偏差(RSD)在0.15%以下。该方法灵敏度高,重复性好,可用于2-甲基哌嗪异构体的质量控制。 相似文献
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高效液相色谱直链淀粉手性固定相拆分奥美拉唑对映体 总被引:1,自引:0,他引:1
建立了奥美拉唑对映体的高效液相色谱拆分方法。使用Chiralpak AD-H手性色谱柱,考察了流动相中极性调节剂的种类和体积分数、流动相中二乙胺体积分数、柱温以及流速对拆分奥美拉唑对映体的影响。确定了最佳拆分条件:流动相为V(正己烷)∶V(异丙醇)∶V(二乙胺)=75∶25∶0.05;流速为0.8 mL/min;检测波长302nm;柱温30℃,计算了奥美拉唑与固定相相互作用的焓变差值Δ(ΔH0)和熵变差值Δ(ΔS0),分别为-2.845 kJ/mol和-6.233 J/(mol.K),所建立的方法简便快速,重复性好,可用于奥美拉唑的质量研究和控制。该研究以(R)-联二萘酚作为包结拆分剂,拆分后的奥美拉唑对映体过量值(ee)可达96.7%以上。通过峰面积的显著差异,考察了在以乙醇或异丙醇为极性调节剂流动相中两对映体的出峰顺序。结果发现,在这两种流动相中出峰顺序是相反的。 相似文献
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结晶原理和色谱原理是拆分手性药物用到的两大主要原理,而高效液相色谱法和模拟移动床(SMB)色谱分离技术是利用色谱原理拆分手性药物的两大重要手段。本研究用高效液相色谱法测定了酮洛芬对映体在Chiralpak AD柱中,以正己烷和乙醇(体积比80∶20)为流动相,多温度下的流出曲线。并以此为基础用拟合度最好的八参数bi-Langmuir模型,运用逆向法来考察该药物对映体在不同温度下,温度对竞争吸附等温线参数的影响,并对3温度下的酮洛芬过载曲线同时拟合,确定出bi-Langmuir中受温度影响的模型参数。 相似文献
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模拟移动床(SMB)色谱分离与纯化的操作过程复杂,对其进行设计与优化需要使用数值模拟方法,准确测定竞争型吸附等温线具有重要意义。采用逆向法确定了25℃下酮洛芬对映体在直链淀粉手性固定相(Chiralpak AD)上的竞争吸附等温线,先用高效液相色谱测得酮洛芬对映体在Chiralpak AD 柱上的过载流出曲线,再通过拟合实验测得的流出曲线确定吸附等温线模型及其参数。研究中采用平衡扩散模型描述酮洛芬对映体在色谱柱上流出的瞬态过程。参数拟合过程中,首先用非支配基因算法(NSGA-Ⅱ)在较广的参数空间内搜索吸附等温线模型参数,再以所得结果作为初值,使用Levenberg-Marquardt 算法(LMA)对参数进一步优化。比较了4种不同竞争吸附等温线模型对实验测得的流出曲线的拟合结果,其中五参数的Bi-Langmuir 模型拟合程度最好。测量了不同进料浓度和进料量条件下的流出曲线,并通过与模型预测结果的对照验证了所确定吸附等温线模型和参数。 相似文献
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纤维素-三(3,5-二甲基苯基氨基甲酸酯)对烯唑醇对映体的直接拆分 总被引:3,自引:2,他引:3
制备了纤维素-三(3,5-二甲基苯基氨基甲酸酯)手性固定相(CDMPC),以正己烷为流动相,添加异丙醇为改性剂,在高效液相色谱上实现了对烯唑醇光学异构体的直接拆分,探讨了改性剂的含量及色谱柱长对拆分效果的影响,从而优化了拆分条件。试验结果显示,流动相中异丙醇含量的减少有利于对映体的拆分,但保留增强;长色谱柱也有利于对映体的分离。使用两色谱柱串连,当流动相中正己烷与异丙醇的比例为95:5时可达到最佳分离效果,分离因子为1.17。 相似文献
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合成了含少量3-(三乙氧基硅)丙基氨基甲酸酯的纤维素3,5-二甲基苯基氨基甲酸酯衍生物(CDMPC),并采用1,2-二(三乙氧基硅基)乙烷(BTSE)为偶联剂,通过溶胶-凝胶法成功制备得到新型硅基杂化手性固定相。该固定相的CDMPC含量达60%,在含有10%氯仿的流动相中保持良好的手性识别性能和机械强度。使用其拆分了多种手性化合物,拆分效果优于商品柱Chiralpak IB,其中对2,2,2-三氟-1-(9-蒽基)乙醇和反式二苯乙烯氧化物对映体的分离选择性分别达到2.99和2.48,表明该类硅基杂化类手性固定相在制备色谱领域中有潜在应用前景。 相似文献
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Enantiomer separation is one of the most important prerequisites for the investigation of environmental enantioselective behavior for chiral pesticides.The enantiomeric separation of three chiral pesticides,indoxacarb,lambda-cyhalothrin,and simeconazole,were studied on cellulose tris-(3,5-dimethylphenyl-carbamate)-coated chiral stationary phase(CDMPC-CSP) using high-performance liquid chromatography under normal phase condition.The effects of chromatographic conditions,such as the mobile phase composition including the concentration and type of alcohol modifiers in hexane,flow rate and column temperature,on enantiomer separation were examined.The thermodynamical mechanism of enantioseparation and chiral recognition mechanism were discussed.Better separation were achieved using 20% n-propanol for indoxacarb,2% iso-butanol for lambda-cyhalothrin,and 20% iso-propanol for simeconazole as modifiers in hexane at 25℃ with the selectivity factor(a) of 1.69,1.82 and 1.70,respectively.The resolution factor(Rs) decreased as the flow rate increased from 0.4 to 1.1 ml·min-1.The retention factor(k’) and selectivity factor for the enantiomers of analytes decreased as temperature increased.The lna-1/T plots for racemic chiral pesticides were linear in the range of 15-35℃ in hexane/iso-propanol and the chiral separation was controlled by enthalpy.Hydrogen bonding,π-π and dipole-dipole interactions between enantiomers and CDMPC-CSP play an important role in chiral identification,and the fitting of the asymmetric portion of solutes in a chiral cavity or channel of the CSP is also important. 相似文献
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Vincenzo Fotia Angela Giorgia Potortì Giovanna Loredana La Torre Giuseppa Di Bella Marcello Saitta 《Journal of the American Oil Chemists' Society》2021,98(11):1035-1043
Enantiomeric separations were performed on five modified polysaccharide-based chiral stationary phases (CSPs) containing cellulose tris(3,5-dimethylphenylcarbamate) (Lux Cellulose-1), cellulose tris(3-chloro-4-methylphenylcarbamate) (Lux Cellulose-2), cellulose tris(4-methylbenzoate) (Lux Cellulose-3), cellulose tris(4-chloro-3-methylphenylcarbamate) (Lux Cellulose-4), amylose tris(5-chloro-2-methylphenylcarbamate) (Lux Amylose-2) by high-performance liquid chromatography and evaporative light scattering detector. A method for direct separation of pairs of sn-1(3)-monoacylglycerols (MAGs) was established using n-hexane/2-propanol as the mobile phase. The washing of CSPs with mobile phases based on n-hexane/2-propanol, containing small amount of acids, improved considerably the efficiency of separations. Racemic mixtures of sn-1(3)-MAGs with different acyl chains could not be directly separated using only one of the columns tested; employing a tandem column system that consisted of a very short silver-loaded column connected downstream with Lux Cellulose-1 the method allowed, for the first time, the separation of four enantiomeric pairs of standard in a single chromatographic run. 相似文献
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M. Isabel Burguete Jean M. J. Fréchet Eduardo García-Verdugo Miroslav Janco Santiago V. Luis Frantisek Svec María J. Vicent Mingcheng Xu 《Polymer Bulletin》2002,48(1):9-15
Summary
Two different families of peptidomimetics have been synthesized and used as chiral selectors for enantioselective chromatography.
The functionalization of compounds with multiple nitrogen atoms allows their use in the preparation of chiral stationary phases
(CSPs), with acrylic or styril comonomers, in both bead and monolithic formats. Some of these separation media, having the
appropriate morphological properties for their use in chromatographic columns, were able to efficiently discriminate enantiomers
of aminoacid derivatives and pharmaceuticals such as Oxazepam.
Received: 24 September 2001/Revised version: 2 January 2002/ Accepted: 21 January 2002 相似文献
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Cecilia Cagliero Barbara Sgorbini Chiara Cordero Erica Liberto Patrizia Rubiolo Carlo Bicchi 《Israel journal of chemistry》2016,56(11-12):925-939
This article deals with enantioselective gas chromatography (Es-GC) utilizing cyclodextrin derivatives as chiral stationary phases (CSPs) for chiral recognition in the flavour and fragrance field. It consists of two main parts. The first one concerns cyclodextrins and their use in Es-GC, and it deals with their introduction and evolution as CSPs in GC, together with some theoretical aspects involved with enantiomeric separation and their consequent influence on routine chiral recognition. The second part reports on the strategy of chiral recognition in routine analysis with cyclodextrin derivatives as CSP, illustrated with examples from the authors’ everyday experiences. This part describes how to identify enantiomers or to measure their excess or ratio determination in complex mixtures; in particular, it discusses the opportunities offered by multidimensional and fast GC techniques, the role of mass spectrometry, and the application of total analysis systems to chiral recognition. 相似文献
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改性环糊精手性毛细管柱的研制及拆分机理 总被引:2,自引:0,他引:2
合成了四种改性 β 环糊精手性固定相 ,对几类手性化合物和芳香异构体进行了拆分 ,并研究了其可能的拆分机理 ,同时对毛细管柱的色谱性能进行了考察。 相似文献