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1.
Rifamycin-capped (3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles (RCD-HPS), a new type of substituted β-cyclodextrin-bonded chiral stationary phase (CSP) for high-performance liquid chromatography (HPLC), have been synthesized by the treatment of bromoacetate-substituted-(3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles (BACD-HPS) with rifamycin SV in anhydrous acetonitrile. The stationary phase is characterized by means of elemental analysis and Fourier-transform infrared spectroscopy. This new CSP has a chiral selector with two recognition sites: rifamycin and β-cyclodextrin (β-CD). The chromatographic behavior of RCD-HPS was studied with several disubstituted benzenes and some chiral drug compounds under reversed-phase HPLC mobile phase conditions. The results show that RCD-HPS has excellent selectivity for the separation of aromatic positional isomers and enantiomers of chiral compounds due to the cooperative functioning of rifamycin and β-CD. 相似文献
2.
Preparation and evaluation of a chiral HPLC stationary phase based on cone calix[4]arene functionalized at the upper rim with l‐alanine units
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《Biomedical chromatography : BMC》2018,32(3)
Here we report a new chiral stationary phase (CSP) immobilized on silica gel based on cone calix[4]arene functionalized at the upper rim with two l ‐alanine units as new chiral selector that has been used in high‐performance liquid chromatography. The CSP was prepared by covalently bonding the allyl groups at the lower rim of calix[4]arene to silica gel by thiol‐ene click chemistry reaction. Elemental analysis of the CSP showed that 120 μmol of chiral selector bonded per gram of silica gel. 1‐Hexene was used for end‐capping of unreacted mercapto groups on silica gel. Since the CSP is chemically bonded to the silica, it can be used in the normal‐phase and reversed‐phase mode and with halogenated solvents as mobile phases, if desired. The chromatographic performance of the CSP was evaluated in the enantioseparation of the 3,5‐dinitrobenzoyl derivatives of some amino acids, diclofop‐methyl and dl ‐mandelic acid. 相似文献
3.
Development of Vancomycin-Capped β-CD-Bonded Silica Particles as Chiral Stationary Phase for LC 总被引:1,自引:0,他引:1
Jia Zhao S. K. Thamarai Chelvi Daphane Tan E. L. Yong Hian Kee Lee Yinhan Gong 《Chromatographia》2010,72(11-12):1061-1066
Vancomycin-capped (3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles (VCD-HPS), a new type of substituted β-cyclodextrin-bonded chiral stationary phase (CSP) for liquid chromatography (LC), have been synthesized by treatment of bromoacetate-substituted-(3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles (BACD-HPS) with vancomycin in anhydrous methanol. The stationary phase is characterized by elemental analysis. This new CSP has a chiral selector with two recognition sites: vancomycin and β-cyclodextrin (β-CD), which can provide multiple interactions with the solutes. The chromatographic performance of VCD-HPS was studied with several disubstituted benzenes and some chiral drug compounds as solutes in reversed-phase LC. The results show that VCD-HPS has excellent selectivity for the separation of aromatic positional isomers and enantiomers of chiral compounds. 相似文献
4.
Bromoacetate‐substituted [3‐(2‐O‐β‐cyclodextrin)‐2‐hydroxypropoxy]propylsilyl‐appended silica particles (BACD‐HPS), an important and useful synthetic intermediate for preparation of novel types of macrocycles‐capped β‐CD‐bonded silica particles including crown ether/cyclam/calix[4]arene‐capped β‐CD‐bonded silica particles, have been prepared and used as chiral stationary phase for HPLC. This synthetic stationary phase is characterized by means of elemental analysis. For the first time, the chromatographic behavior of BACD‐HPS was systematically evaluated with several disubstituted benzenes and some chiral drug compounds under both normal and RP conditions in HPLC. The results show that BACD‐HPS has excellent selectivity for the separation of aromatic positional isomers and chiral isomers of some drug compounds when used as stationary phase in HPLC. 相似文献
5.
合成了两种新型的杯(4)芳烃衍生物:5-1′,1′-二甲基十一烯氧基苯基甲基-11,17,23-三-1,1-二甲基乙基-25,26,27,28-四苄氧基杯(4)芳烃C(4)TB)及5-1′,1′-二甲基十一烯氧基苯基甲基-11,17,23-三-1′,1′-二甲基-25,26,27,28-四乙氧羰甲氧基(C(4)TECM)其结构经元素分析IR,^1HNMR,MS的数据证实,分别将其与OV-1701固 相似文献
6.
Wenfen Zhang Yongming Zhang Guangrui Zhang Xin Ba Shaige Xia Wuduo Zhao Dan Yin Shusheng Zhang 《Journal of separation science》2019,42(7):1374-1383
A new water‐soluble tetra‐proline‐modified calix[4]arene‐bonded silica stationary phase was prepared straightforwardly by an indirect method and characterized by elemental analysis, energy dispersive Spectrometry, solid‐state 13C NMR spectroscopy, Fourier‐transform infrared spectroscopy, and thermogravimetric analysis. Due to the simultaneous introduction of polar tetra‐proline and nonpolar calix[4]arene, the developed column possessing a double retention mode of reverse‐phase liquid chromatography and hydrophilic interaction liquid chromatography. A series of hydrophobic and hydrophilic test samples, including nucleosides and nucleotides, amines, monosubstituted benzenes, chiral compounds, and phenols, were used to evaluate the developed stationary phase. A rapid separation capability, high separation efficiency, and selectivity were achieved based on the multiple interactions between solutes and tetra‐proline‐modified calix[4]arene‐bonded silica stationary phase. Moreover, the developed stationary phase was further used to detect and separate hexamethylenetetramine in rice flour. All the results indicated the potential merits of the developed stationary phase for simultaneous separation of complex hydrophobic and hydrophilic samples with high selectivity. 相似文献
7.
Gong Y Xiang Y Yue B Xue G Bradshaw JS Lee HK Lee ML 《Journal of chromatography. A》2003,1002(1-2):63-70
Two bonded chiral stationary phases (CSPs), 8-aminoquinoline-2-ylmethyl- and 8-aminoquinoline-7-ylmethyl-diaza-18-crown-6-capped [3-(2-O-beta-cyclodextrin)-2-hydroxypropoxy]propylsilyl silica particles (non-porous, 1.5 microm), have been prepared and evaluated using capillary liquid chromatography at high pressures (> or = 8000 p.s.i.). High column efficiency (up to 400 000 plates m(-1)) was achieved for chiral separations. These CSPs with two recognition sites, i.e. substituted-diaza-18-crown-6 and beta-cyclodextrin combined with high chromatographic efficiency provide good resolution of a variety of enantiomers and positional isomers in relatively short times under reversed-phase conditions. After inclusion of a Ni (II) ion from the mobile phase, the positively charged crown ether-capped beta-cyclodextrin facilitates specific static, dipolar, and host-guest complexation interactions with solutes. 相似文献
8.
《Analytical letters》2012,45(9):1543-1551
Abstract The synthesis of a new type of chiral stationary phase, prepared from triethoxysilyl derivatives of calixarenes, and by the chemical immobilisation of these chiral molecular baskets to 3μm silica particles, is reported. Specifically, a silica-bonded calix[4]arene, funcrionalised at the lower rim with L-(-)-ephedrine, is prepared and packed into a short LC column for rapid chiral separations. Using reversed phase conditions and high flow rate, such new phases based on funcrionalised calixarenes are applicable to chiral aromatic and non-aromatic solutes and are capable of resolving the enantiomers of R(-) and S(+)-1-phenyl-2,2,2-trifluoroethanol in less than 45 seconds. 相似文献
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《Journal of separation science》2018,41(9):1903-1912
We report the synthesis and enantioseparation characteristics of two novel covalently immobilized deoxycholic acid derivatives as chiral stationary phases for high‐performance liquid chromatography. In the structure of the first stationary phase, the 3‐position of deoxycholic acid is substituted with a 3,5‐dinitrophenylcarbamoyl group and the second one has an additional calix[4]arene attached to the carboxylic group of the deoxycholic acid. The chromatographic performance of the stationary phases was evaluated with enantioseparation of N‐(3,5‐dinitrobenzoyl)‐dl ‐leucine, N‐(3,5‐dinitrobenzoyl)‐dl ‐valine, omeprazole, diclofop‐methyl, dl ‐mandelic acid and (RS)‐pregabalin. Comparison of the performance characteristics of the prepared chiral stationary phases provided evidence for the active involvement of the calix[4]arene unit in the chiral recognition process. Both stationary phases are chemically bonded to the silica and can be used in both normal‐phase and reversed‐phase modes. 相似文献
13.
Serkan Erdemir Mustafa Yilmaz 《Journal of inclusion phenomena and macrocyclic chemistry》2012,73(1-4):141-150
Two novel chiral di- and tri-amide derivatives of p-tert-butylcalix[4]arene were synthesized by (R)-(+)-1-Phenylethylamine via convenient reactions and then immobilized on aminopropyl functionalized silica particles. The prepared chiral calix[4]arenes and their silica polymers (Calix-SP1 and Calix-SP2) were characterized using 1H NMR, 13C NMR, FT-IR, and thermal and elemental analysis techniques. 相似文献
14.
Summary Two new kinds of calix[4]arene derivatives, 5, 11, 17, 23-tetra-tert-butyl-25,27-bis(isopropylcarbamoyl-methoxy)-26,28-diundecenyloxy
calix[4]arene (C[4]A) and 25,27-dibutoxy-5, 11, 17, 23-tetra-tert-butyl-26,28-diundecenyloxy calix[4]arene (C[4]B0, are prepared
and then are polymized by two different processes. Three calix[4]arene polysiloxane stationary phases for capillary gas chromatography
are obtained. Their chromatographic characteristics, including column efficiency, polarity, selectivity, glass-transition
temperature and thermal stability are studied. Retention mechanisms are also discussed. 相似文献
15.
Hasalettin Deligöz 《Journal of inclusion phenomena and macrocyclic chemistry》2002,43(3-4):285-289
In this study, seven new compounds p-(4-butyl-phenylazo)calix[6]arene(1), p-(4-(phenylazo)phenylazo)calix[6]arene (2),p-(4-hydroxyphenylazo)calix[6]arene (3),p-{4-[N-(thiazol-2-yl)sulfamoyl]phenylazo\}calix[6]arene(4), p-(4-acetamidophenylazo)calix[6]arene (5),p-(thiazol-2-ylazo)calix[6]arene (6) andp-(2-sulfanylphenylazo)calix[6]arene (7) have been synthesizedfrom calix[6]arene by diazo coupling with the corresponding aromaticamines. UV-Vis, IR, 1H and 13C NMR spectral data have been used to elucidate the structures of the compounds elemental analyses 相似文献
16.
合成了一种新的对-叔丁基杯[8]芳烃的高效液相色谱键合固定相,考察了多环芳烃、苯甲酸酯、邻苯二甲酸酯、苯的单官能团取代物在该键合相上的反相液相色谱保留行为,并以甲醇-水作为流动相分离了氨基苯酚的邻、间、对取代位置异构体.研究结果发现,该键合相具有明显的反相特征,并讨论了可能的分离机理. 相似文献
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A. R Hajipour S. Habibi A. E. Ruoho 《Journal of inclusion phenomena and macrocyclic chemistry》2011,69(1-2):107-117
The novel chiral polymeric compounds containing more than one calix[4]arene have been synthesized by reacting a new calix[4]arene diamine derivative with two chiral monomers. These newly prepared compounds were studied by extraction of toxic heavy metal (Cu2+, Co2+, Cd2+, Hg2+), silver and alkali metal (Na+, K+) cations from aqueous phase. It was observed that the resulting calixarene-based polymers have a good complexing ability towards silver, alkali metal and toxic heavy metal cations. 相似文献
19.
In the present study, the synthesis and liquid phase extraction properties towards some amino acid methylesters and amino alcohols of Schiff base and amino alcohol substituted calix[4]arene are reported. The Schiff base substituted calix[4]arene 5 has been synthesized via condensation reaction involving 5,17-diformyl-11,23-di-tert-butyl-25,27-di[3-(4-formylphenoxy)propoxy]-26,28 dihydroxycalix[4]arene 4 and (R)-(?)-2-phenylglycine methyl ester in CHCl3:MeOH. To give the amino alcohol substituted calix[4]arene 6, the synthesized chiral compound 5 was reduced by LiAlH4. The new chiral Schiff base and amino alcohol derivatives of calix[4]arene have been characterized by a combination of FT-IR, 1H NMR, 13C NMR, FAB-MS and elemental analysis. Also, the extraction behaviors of 5 and 6 towards some selected amino acid methylesters and amino alcohols have been studied by liquid–liquid extraction. 相似文献
20.
LiJunHE ShiJunSHAO YongGUO HuaJiaoMA XiaLIU ShengXiangJIANG 《中国化学快报》2003,14(9):946-947
Octadecylsilanized silica (ODS) was coated with meso-octarnethylcalix[4]pyrrole to obtain a novel calix[4]pyrrole containing stationary phase for HPLC. Compared to ODS, the new stationary phase showed a relatively large retention and an improved separation for phenolic compounds and organic anions, using pure water as mobile phase. The results can be ascribed to the interaction between analytes and calix[4]pyrrole. 相似文献