共查询到19条相似文献,搜索用时 346 毫秒
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高效液相色谱(HPLC)被广泛认为是分离制备光学纯单一对映体的最有效方法。在高效液相色谱手性拆分中,手性固定相(CSP)的性能直接影响到色谱柱的手性分离能力。在众多手性固定相中,键合型手性固定相具有溶剂耐受性好,分离模式灵活等优点,已经发展成为一类重要的手性固定相。本文通过两步化学反应合成了新型的光学活性丙烯酰胺衍生物--(S)-1-丙烯酰-2-(N-苯基甲酰胺基)吡咯烷((S)-APACP),采用核磁共振氢谱表征了(S)-APACP的化学结构;通过3步化学反应制备了键合型聚丙烯酰胺衍生物手性固定相,采用热重分析法表征了聚合物的键合量,采用HPLC评价了键合型手性固定相的识别能力,分析了影响其手性识别能力的因素。研究结果表明,APACP聚合物成功地键合到硅胶表面制备了具有良好溶剂耐受性的键合型手性固定相,其聚合物键合量为10.2%~11.8%,该键合型手性固定相对若干种对映体显示了较好的手性识别能力。 相似文献
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手性金属簇合物的合成、结构表征及其反应 总被引:2,自引:0,他引:2
用潜手性羰基簇合物 ( μ3 S)RuCo2 (CO) 9( 1 )与阴离子金属交换试剂Na[M (CO) 3C5 H4C(O)R][R =H ,CH3,C6 H5 ,C6 H4C(O)OCH3;M =Mo ,W ]在四氢呋喃中回流反应 ,生成一系列新的由四个不同原子组成的不对称四面体簇合物 ( μ3 S)RuCoM (CO ) 8CpCOR .研究了簇合物 ( μ3 S)RuCoMo(CO) 8CpCOCH3的还原反应 .对合成的所有化合物进行了IR、1HNMR、C/H元素分析 ,测定了簇合物( μ3 S)RuCoMo(CO) 8CpCOC6 H5 的单晶结构 . 相似文献
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以单分散亲水性交联聚甲基丙烯酸环氧丙酯-甲基丙烯酸乙二醇双酯(PGMA/EDMA)树脂为载体,制备新型L-羟脯氨酸聚合物键合高效手性配体交换固定相。该固定相在配体交换分离模式下,以0.2mol/LNaAc和0.1mmol/LCu(Ac)2水溶液(pH5.2)为流动相,柱温为30℃~50℃,对衍生和非衍生的D,L-氨基酸和α-羟基酸等9种手性化合物进行了高效液相色谱拆分。详细考察了流动相pH值、温度、流速和进样量对手性分离的影响,选择了合适的色谱分离条件。结果表明,所拆分的9种手性化合物,有5种手性化合物能得到基线分离,最好的分离因子α=2.32。 相似文献
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Han Xiaoqian Liu Yueqi Zhang Yuhua Zhang Weiqiang Li Yongmin Chen Liren 《Chromatographia》2002,56(5-6):319-322
Summary Amylose tris(phenylcarbamate) (ATPC) coated on a small particle silica gel was prepared. This ATPC chiral stationary phase
(ATPC-CSP) was found to be useful for the enantiomeric separation of some novel chiral tetrahedrane-type clusters. Moreover,
the influence of mobile phase modifier and of the structure of chiral tetrahedrane-type clusters on the chiral separation
and retention were investigated. The results suggest that not only the structure and concentration of alcohol in mobile phase,
but also the subtle structural differences in racemates can have a pronounced effect on enantiomeric separation and retention. 相似文献
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In the present work, an amylose tris(3,5-dimethylphenylcarbamate) (ADMPC) chiral stationary phase (CSP) was prepared by coating ADMPC on small-particle silica gel. This ADMPC-CSP was for the first time successfully applied to separate a series of novel chiral metal tetrahedrane-type clusters. Furthermore, the influence of a mobile-phase modifier (various alcohols added in the mobile phase), including its concentration and structure, and the structures of the clusters on the chiral separation and retention was investigated. The results suggest that not only the structure and concentration of alcohol in the mobile phase, but also the subtle structural differences in racemate can have a pronounced effect on the enantiomeric separation and retention. 相似文献
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Green high‐performance liquid chromatography enantioseparation of lansoprazole using a cellulose‐based chiral stationary phase under ethanol/water mode
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Rosella Ferretti Leo Zanitti Adriano Casulli Roberto Cirilli 《Journal of separation science》2016,39(8):1418-1424
A simple and environmentally friendly reversed‐phase high‐performance liquid chromatography method for the separation of the enantiomers of lansoprazole has been developed. The chromatographic resolution was carried out on the cellulose‐based Chiralpak IC‐3 chiral stationary phase using a green and low‐toxicity ethanol‐aqueous mode. The effects of water content in the mobile phase and column temperature on the retention of the enantiomers of lansoprazole and its chiral and achiral related substances have been carefully investigated. A mixed‐mode hydrophilic interaction liquid chromatography and reversed‐phase retention mechanism operating on the IC‐3 chiral stationary phase allowed us to achieve simultaneous enantioselective and chemoselective separations in water‐rich conditions. The enantiomers of lansoprazole were baseline resolved with a mobile phase consisting of ethanol/water 50:50 without any interference coming from chiral and achiral impurities within 10 min. 相似文献
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应用纤维素三(3,5-二甲基苯基氨基甲酸酯)(cellulose tris (3, 5- dimethylphenylcarbamate,CDMPC)手性固定相对两种新型金属簇合物进行了拆分,通过流动相组成、流速和样品溶剂等条件对拆分影响的考察进行了拆分条件的优化。实验结果表明,簇合物1和簇合物2分别在含乙醇V(hexane)∶V(ethanol)=95∶5)和异丙醇(V(hexane)∶V(2-propanol)=90∶10)的流动相中得到了较好的拆分,将样品溶解在和流动相组成相近的溶剂中更利于簇合物拆分,簇合物配体结构对簇合物在固定相上的保留和拆分有重要的影响。 在优化条件下,2种金属簇合物分离度均达到1.5以上。 相似文献
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应用纤维素三(3,5-二甲基苯基氨基甲酸酯)(CDMPC)手性固定相对2种羰基钌金属簇合物进行了拆分,通过流动相组成、流速和样品溶剂等条件对拆分影响的考察对拆分条件进行了优化。实验结果表明,簇合物1和簇合物2分别在含乙醇(V(hexane):V(ethanol)=95:5)和异丙醇(V(hexane):V(2-propanol)=90:10)的流动相中得到了较好的拆分,将样品溶解在和流动相组成相近的溶剂中更利于簇合物拆分,簇合物配体结构对簇合物在固定相上的保留和拆分有重要的影响。在优化条件下,2种金属簇合物分离度均达到1.5以上。 相似文献
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高效液相色谱-串联质谱法结合多糖衍生物手性固定相拆分氰戊菊酯 总被引:1,自引:0,他引:1
建立了以多糖衍生物为手性固定相的高效液相色谱-串联质谱(HPLC-MS/MS)直接拆分氰戊菊酯对映体的方法。在反相液相色谱条件下,考察了手性固定相的种类、流动相组成、柱温、流速对氰戊菊酯4个立体异构体分离的影响。同时,利用热力学方法对氰戊菊酯的立体异构体与固定相之间的色谱保留和分离的热力学机理进行了探讨。结果表明:采用Lux Cellulose-3(纤维素-三(4-甲基苯甲酸酯))手性色谱柱,在以流动相为乙腈-水(5 mmol/L甲酸铵)=(55:45,V:V)流速0.4 mL/min,柱温30℃的条件下,可在14 mins内实现氰戊菊酯4个立体异构体的基线分离。拓展了HPLC-MS/MS在菊酯类手性农药对映体分离及检测上的应用。 相似文献
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Enantioseparation tuned by solvent polarity on a β‐cyclodextrin clicked chiral stationary phase
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The efficient enantioseparation of 26 racemates has been achieved with the perphenylcarbamoylated cyclodextrin clicked chiral stationary phase by screening the optimum composition of mobile phase in high‐performance liquid chromatography. The chromatographic results indicate that both the retention and chiral resolution of racemates are closely related to the polarity of the mobile phases and the structures of analytes. The addition of alcohols can significantly tune the enantioseparation in normal‐phase high‐performance liquid chromatography. The addition of methanol and the ratio of ethanol/methanol or isopropanol/methanol played a key role on the resolution of flavonoids in ternary eluent systems. The chiral separation of flavonoids with pure organic solvent as mobile phase indicates the preferential order for chiral resolution is methanol>ethanol>isopropanol>n‐propanol>acetonitrile. 相似文献