研究了在反相高效液相色谱模式下,基于点击化学的β-环糊精手性固定相对苯并恶嗪类对映体的手性分离情况.考察了流动相中有机改性剂的类型和比例、缓冲盐的浓度和pH值对分离的影响.考察结果表明:乙腈作为有机改性剂比甲醇更有利于苯并恶嗪对映体的分离;乙酸三乙胺缓冲盐体积分数从0.1%增大到1.0%时,苯并恶嗪对映体的保留时间和分离度都随之减小,在pH4.1时苯并恶嗪对映体具有最大分离度.因此确定乙腈和体积分数为0.1%的乙酸三乙胺缓冲盐流动相(pH 4.1)为最佳分离条件.分离机理研究结果表明,固定相和样品之间的包容络合相互作用以及样品和固定相之间的氢键作用,是样品得以分离的基础.本研究为进一步深入研究β-环糊精固定相提供了实验基础,同时也证明了点击化学在手性环糊精固定相制备中具有极大潜力.
参考文献
[1] | Fanali S.J Chromatogr A,1996,735:77 |
[2] | Yashima E J.J Chromatogr A,2001,906:105 |
[3] | Park J Y,Cho H S,Hyun M H.Chirality,2011,23:E16 |
[4] | Michishita T,Franco P,Zhang T.J Sep Sci,2010,33:3627 |
[5] | Jiang H L,Li Y H,Pelzer M,et al.J Chromatogr A,2008,1192:230 |
[6] | Loukotková L,Tesa(r)ová E,Bosáková Z,et al.J Sep Sci,2010,33:1244 |
[7] | Zhou Z M,Li X,Chen X P,et al.Talanta,2010,82:775 |
[8] | Ha J J,Choi H J,Jin J S,et al.J Chromatogr A,2010,1217:6436 |
[9] | Zaidi S A,Han K M,Hwang D G,et al.Electrophoresis,2010,31:1019 |
[10] | Cho H S,Choi H J,Hyun M H.J Chromatogr A,2009,1216:7446 |
[11] | Zheng J,Bragg W,Hou J G,et al.J Chromatogr A,2009,1216:857 |
[12] | Solms J,Engli R H.Helv Chim Acta,1965,48:1225 |
[13] | Fujimura K,Ueda T,Ando T.Anal Chem,1983,55(3):446 |
[14] | Kawaguchi Y,Tanaka M,Nakae M,et al.Anal Chem,1983,55:1852 |
[15] | Armstrong D W.US Patent,4539399,1985-09-03 |
[16] | Fujimura K,Kitagawa M,Takayanagi H,et al.J Liq Chromatogr,1986,9:607 |
[17] | Armstrong D W,Stalcup A M,Hilton M L,et al.Anal Chem,1990,62:1610 |
[18] | Poon Y F,Muderawan I W,Ng S C.J Chromatogr A,2006,1101:185 |
[19] | Zhang L F,Wong Y C,Chen L,et al.Tetrahedron Lett,1999,40:1815 |
[20] | Kolb H C,Finn M G,Sharpless K B.Angew Chem Int Ed,2001,40:2004 |
[21] | Fu C M,Shi H Y,LiZW,et al.Chinese Journal of Analytical Chemistry(付春梅,石宏宇,李章万,等.分析化学),2010,38(7):1011 |
[22] | Guo Z M,Lei A W,Liang X M,et al.Chem Commun,2006,43:4512 |
[23] | Wang Y,Ong T T,Li L S,et al.J Chromatogr A,2009,1216:2388 |
[24] | Wang Y,Xiao Y,Tan T T Y,et al.Tetrahedron Lett,2008,49:5190 |
[25] | Zhang Y P,Guo Z M,Ye J X,et al.J Chromatogr A,2008,1191:188 |
[26] | Zhao Y Y,Guo Z M,Xue X Y,et al.Chinese Journal of Chromatography(赵艳艳,郭志谋,薛兴亚,等.色谱),2011,29(9):885 |
[27] | Li X,Zhou Z M,Meng Z H.Chinese Journal of Chromatography(李霞,周智明,孟子晖.色谱),2010,28(4):413 |
[28] | Lai X H,Ng S C.J Chromatogr A,2004,1059:53 |
[29] | Muderawan W I,Ong T T,Ng S C.J Sep Sci,2006,29:1849 |
[30] | Wang Y,Young D J,Tan T T Y,et al.J Chromatogr A,2010,1217:7878 |
[31] | Wang Y,Young D J,Tan T T Y,et al.J Chromatogr A,2010,1217:5103 |
[32] | Lai X H,Tang W H,Ng S C.J Chromatogr A,2011,1218:5597 |
[33] | Wang Y,Chen H,Xiao Y,et al.Nat Protoc,2011,6(7):935 |
[34] | Rueping M,Antonchick A P,Theissmann T.Angew Chem Int Ed,2006,45:6751 |
[35] | Liu Z Q,Chen Y W.Tetrahedron Lett,2009,50:3790 |
[36] | Miao H,Guo H Y.Chinese Journal of Pharmaceuticals(苗华,郭慧元.中国医药工业杂志),1994,25:185 |
[37] | Yu Z W.[PhD Dissertation].Lanzhou:Lanzhou Institute of Chemical Physics,Chinese Academy of Sciences(于兆文.[博士学位论文].兰州:中国科学院兰州化学物理研究所),1999 |
[38] | McCalley D V.J Chromatogr A,2010,1217:858 |
[39] | Dalgliesh C E.J Chem Soc,1952:3940 |
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