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利用二硝基苯甲酰-苯基甘氨酸型手性固定相直接拆分丙卡特罗药物对映体 总被引:6,自引:0,他引:6
用手性源(R)-苯基甘氨酸,采用非对称合成方法制备了3,5-二硝基苯甲酰-(R)-苯基甘氨酸手性固定相(DNB-PG CPS),利用它直接拆分了丙卡特罗药物的部分对映体,取得了良好的拆分效果。以不同比例的异丙醇-正己烷(体积比分别为20∶80,10∶90,5∶95,2∶98)为流动相,对丙卡特罗进行了拆分,其分离因子α的范围为1.54-1.67。此外,还测试了不同流动相组成对分离效果的影响,考察了液固吸附色谱保留值方程lnk=a+cC b+blnC b中保留因子k和分离因子α与强极性洗脱剂组分b的浓度C 相似文献
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苯丙醇对映体在酰胺型手性固定相上的分离 总被引:2,自引:0,他引:2
对于手性对映体苯丙醇在3种Pirkle型手性固定相(CSP)Whelk-O 1、DNB-Leu和DNB-Pg上直接分离进行了研究.考察了流动相极性以及温度对分离的影响,发现在常用的范围内无法获得分离,仅有Whelk-O1在流动相极性的极端条件下(正己烷/异丙醇=99.5/0.5,V/V)能够被直接分离.在较低温度0 ℃和流速1 mL/min的优化条件下能获得基线分离.用旋光检测器与液相色谱串联的方式确定了手性拆分结果,并确定了(-)苯丙醇优先洗脱的顺序.针对这种流动相极性极端条件下的分离,结合有关理论,进一步探讨了分离机理. 相似文献
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建立并优化了高效液相色谱手性固定相分离富马酸比索洛尔对映体的方法。使用直链淀粉手性固定相(Chiralpak AD-H柱)在正相条件下拆分了富马酸比索洛尔对映体,考察了达到最佳分离效果时,流动相中极性调节剂的组分、流动相中三乙胺的体积分数以及柱温对富马酸比索洛尔对映体拆分影响。流动相为正己烷/乙醇/三乙胺(90/10/0.1,V/V/V),流速1.0 mL/min,紫外检测波长270 nm,柱温30℃时,两种异构体能达到较好的基线分离,并且不对称合成的(S)-富马酸比索洛尔和(R)-富马酸比索洛尔两种异构体产品,对映体过量(e.e.)均高于99.0%,在此色谱条件下的色谱图峰形良好。方法可广泛用于跟踪手性比索洛尔富马酸盐的合成过程分析和质量控制。 相似文献
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采用多糖类手性色谱柱,建立了(2-戊基-3-苯基-2,3环氧丙烷基)二苯基磷酸酯对映体的高效液相色谱手性拆分方法。考察了手性柱类型、流动相组成、流速、柱温等对手性拆分的影响,并对分离机制进行了探讨。结果表明,采用Chiralpak AS-H柱(250×4.6mm,i.d.,5μm),以正己烷-异丙醇(85∶15,V/V)为流动相,在柱温25℃,流速1.0mL/min,检测波长210nm的条件下,(2-戊基-3-苯基-2,3环氧丙烷基)二苯基磷酸酯对映体能达到完全分离,且稳定性和重复性好。该方法也适用于(2-戊基-3-苯基-2,3环氧丙烷基)二苯基磷酸酯类似物的手性拆分。 相似文献
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使用Chiralpak IC(纤维素-三(3,5-二氯苯基氨基甲酸酯)共价键合硅胶)手性柱,建立了采用手性固定相高效液相色谱拆分6种 α -芳基萘满酮类衍生物对映体的方法。考察了流动相中有机改性剂的种类和比例、柱温和流速对对映体分离的影响。结果显示6种化合物在异丙醇为改性剂的条件下均可获得较高的对映体分离度。热力学研究表明6种化合物对映体的手性拆分过程均受焓驱动影响,且低温有利于对映体分离。最终推荐分离化合物Ⅰ对映体的流动相是正己烷-异丙醇(90:10,v/v);分离化合物Ⅱ、Ⅲ、Ⅳ对映体的流动相是正己烷-异丙醇(99:1,v/v);分离化合物Ⅴ对映体的流动相是正己烷-异丙醇(85:15,v/v);分离化合物Ⅵ对映体的流动相是正己烷-异丙醇(80:20,v/v)。柱温为25℃,流速为1.0 mL/min。6种化合物对映体均可在Chiralpak IC手性固定相上得到完全分离,证明该色谱柱对6种化合物具有较高的对映体选择性。 相似文献
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高效液相色谱手性固定相法拆分阿折地平对映体 总被引:2,自引:0,他引:2
建立了阿折地平对映体的高效液相色谱拆分方法。采用Chiralpak AD-H (250 mm×4.6 mm, 5.0 μm, Daicel公司)手性色谱柱在正相条件下直接拆分阿折地平对映体,考察了固定相种类、流动相组成及柱温等对阿折地平对映体分离的影响。确定了最佳的拆分条件: 流动相为正己烷-异丙醇(90:10, v/v),流速为0.8 mL/min,检测波长为254 nm;柱温为20 ℃;在此条件下阿折地平对映体的分离度为3.3。该法简单快速,重现性好。 相似文献
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Srinivas NR 《Biomedical chromatography : BMC》2004,18(10):759-784
The field of chiral separations had a modest beginning some two decades ago. However, due to rapid technological advancement coupled with simultaneous availability of innovative chiral stationary phases and novel chiral derivatization agents, the field of chiral separations has now totally outpaced many other separation fields. Keeping pace with rapid changes in the field of chiral separations, investigators continue to add stereoselective pharmacokinetic, pharmacodynamic, pharmacologic and toxicological data of new and/or marketed racemic compounds to the literature. Examination of the evolution of chiral separations suggests that in the beginning many investigators attempted to separate and quantify a single pair of enantiomers, adopting either direct (separation made on a chiral stationary phase) or indirect (separation made following precolumn conversion of enantiomers to corresponding diastereomers) approaches. However, more recent trends in chiral separations suggest that investigators are attempting to separate and quantify multiple pairs of enantiomers with available technologies. Added to this, some interesting trends have been observed in many of the recently reported chiral applications, including preferences regarding internal standard selection, mobile phase contents and composition, sorting out issues with mass spectrometric detection, determination of elution order, analytical manipulations of metabolite(s) without reference standards and addressing some specificity-related issues. This review mainly focuses on chiral separations involving multiple chiral analytes and attempts to justify the need for such chiral separations involving multiple analytes. In this context, several cases studies are described on the utility and applicability of such chiral separations under discrete headings to provide an account to the readership on the implications of such tasks. The topics of case studies covered in this review include: (a) therapy markers--differentiation from drug abuse and/or applicability in forensics; (b) role in pharmacogenetic/polymorphic evaluation; (c) monitoring and understanding the role of parent and active metabolite(s) in clinical and preclinical investigations; (d) exploration on the pharmacokinetic utility of an active chiral metabolite vis-a-vis the racemic parent moiety; (e) understanding the chirality play in delineating peculiar toxic effects; (f) exploration of chiral inversion phenomenon, and understanding the role of stereoselective metabolism. For the further benefit of readership, some select examples (n = 19) of the separation of multiple chiral analytes with appropriate information on chromatography, detection system, validation parameters and applicable conclusion are also provided. Finally, the review covers some useful considerations for method development involving multiple chiral analytes. 相似文献
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采用高效液相色谱法,在自制的纤维素-三(3,5-二甲基苯基氨基甲酸酯)(ATEO-OD)、纤维素-三(4-甲基苯基氨基甲酸酯)(ATEO-OG)和纤维素-三(4-甲基苯基甲酸酯)(ATEO-OJ)3种手性柱上对16种不同结构的手性化合物进行了拆分和比较.试验结果表明:16个手性样品在这3种手性固定相上分别获得了不同程度的拆分,A TEO-OD对所分析样品具有更好的手性识别能力,ATEO-OG和ATEO-OJ的手性识别能力相当. 相似文献
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Federica Ianni Lucia Pucciarini Andrea Carotti Serena Natalini Gulnara Z. Raskildina Roccaldo Sardella Benedetto Natalini 《Journal of separation science》2019,42(1):21-37
Chiral ligand‐exchange chromatography is one of the elective strategies for the direct enantioresolution of small chelating compounds: amino acids, diamines, amino alcohols, diols, small peptides, etc. Unlike other methods, the interaction between chiral selector and analyte enantiomers is mediated by a cation, thus producing diastereomeric ternary complexes. Two main approaches are conventionally applied in chiral ligand‐exchange chromatography. The first relies upon chiral stationary phases where the chiral selector is either covalently immobilized or physically adsorbed onto suitable packing materials (coated phases). In the second approach, chiral molecules are added to the eluent, thus generating chiral eluent systems. Among the advantages of chiral ligand‐exchange chromatography, the generation of UV/vis‐active metal complexes, and the use of commercially available or easy‐to‐synthesize chiral selectors, in combination to rather inexpensive achiral columns for coated phases and chiral eluents, are noteworthy. Besides amino acids and amino alcohols, other species have proven suitable for chiral ligand‐exchange chromatography applications. Recently, the use of either chiral ionic liquids or micellar liquid chromatography systems as well as the successful off‐column formation of diastereomeric complexes have expanded the selectivity profiles and application fields. All of these issues are touched in the review, shedding light to the contributions appeared in the last decade. 相似文献
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手性污染物对映体尽管具有相似的物理化学性质,但在环境中的吸附、转移、降解等过程往往存在一定差异。生态安全问题与人类健康密切相关,因此,对手性环境污染物进行对映体水平上的分离分析是十分重要的研究课题。目前,国内外对环境中的手性污染物已开展了相关研究,然而全面评述相关分析测定方法的新进展鲜有报道。本文主要对环境中手性污染物的种类以及近5年环境中手性污染物的分析检测技术如液相色谱-质谱联用法、气相色谱-质谱联用法、毛细管电泳法、超临界流体色谱-质谱联用法等进行了归纳、综述和展望,为后续手性污染物的分析检测提供依据和参考。 相似文献
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Qing‐You Zhang Li‐Zhuang Xu Jing‐Ya Li Dan‐Dan Zhang Hai‐Lin Long Ji‐Yan Leng Lu Xu 《Journal of Chemometrics》2012,26(10):497-508
Chiral compounds are very important in drug development, organic synthesis, materials science, toxicology, or environmental chemistry. Therefore, for creating new drugs, several methods have been suggested in recent years. In several laboratories in the world, some new methods for the derivations of the parameters were constructed and used for studies on quantitative structure–activity/property relationships of chiral molecules. The algorithms reviewed in this paper involve Zargeb group chiral indices, chiral molecular connectivity index, chiral topological charge index, chiral Am index, chiral indices based on the matrixes, chiral indices based on chiral product, conformation‐independent chirality code, conformation‐dependent chirality code, quantitative two‐dimensional chirality degrees of benzenoids, and so on. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献