β-环糊精衍生物手性固定相的制备及其在毛细管电色谱-质谱中的应用
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摘要
通过对β-环糊精进行化学修饰,得到含乙烯基的β-环糊精(UPA-β-CD),并以UPA-β-CD为功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,运用原位聚合法制备了新型毛细管电色谱整体柱。优化制柱条件,对整体柱固定相进行红外光谱、扫描电子显微镜表征。结果表明,所制备的固定相成功键合到毛细管内,并形成复杂的孔隙结构。在毛细管电色谱-质谱(CEC-MS)模式下对盐酸奥昔布宁和盐酸苄丝肼两种手性药物对映体进行拆分。优化分离条件下,两种手性药物均达到基线分离,其分离度RS分别为1.76和2.12。
The vinyl group-containing β-cyclodextrin(UPA-β-CD)was obtained by chemical modification ofβ-cyclodextrin.And then a new capillary electrochromatography column was prepared by in situ polymerization using UPA-β-CD as the functional monomer,ethylene glycol dimethacrylate(EDMA)as crosslinking agent.The preparation conditions of the monolithic column were optimized and the stationary phase was characterized by infrared spectroscopy and scanning electron microscopy.The results showed that the prepared stationary phase was successfully bonded into the capillary and formed the complex pore structure.The enantiomers of two chiral drugs(oxybutynin hydrochloride and benserazide hydrochloride)were separated by capillary electrochromatography-mass spectrometry.The chiral drugs reached the baseline separation under the optimal chromatographic conditions,and the resolutions were 1.76 and 2.12,respectively.
The vinyl group-containing β-cyclodextrin(UPA-β-CD)was obtained by chemical modification ofβ-cyclodextrin.And then a new capillary electrochromatography column was prepared by in situ polymerization using UPA-β-CD as the functional monomer,ethylene glycol dimethacrylate(EDMA)as crosslinking agent.The preparation conditions of the monolithic column were optimized and the stationary phase was characterized by infrared spectroscopy and scanning electron microscopy.The results showed that the prepared stationary phase was successfully bonded into the capillary and formed the complex pore structure.The enantiomers of two chiral drugs(oxybutynin hydrochloride and benserazide hydrochloride)were separated by capillary electrochromatography-mass spectrometry.The chiral drugs reached the baseline separation under the optimal chromatographic conditions,and the resolutions were 1.76 and 2.12,respectively.
引文
[1]Zhang S,Wang H,Tang J,et al.Analytical Methods,2014,6(7):2034.
[2]Rezanka P,NavrtilovK,Rezanka M,et al.Electrophoresis,2014,35(19):2701.
[3]SHEN H M,JI H B,WU H K,et al.Chinese Journal of Organic Chemistry(沈海民,纪红兵,武宏科,等.有机化学),2014,34(8):1549.
[4]Mik2ík I.Journal of Separation Science,2017,40(1):251.
[5]BAI Q.Chinese Journal of Chromatography(白泉.色谱),2015,33(11):1117.
[6]LIN Z A,PANG J L,HUANG H,et al.Chinese Journal of Chromatography(林子俺,庞纪磊,黄慧,等.色谱),2010,28(3):273.
[7]MoravcovD,Rantamki A H,Du2a F,et al.Electrophoresis,2016,37(7-8):880.
[8]Grange R L,Evans P A.Journal of the American Chemical Society,2014,136(34):11870.
[9]FENG F,TANG L,XU Z G,et al.Chemical Reagents(冯锋,汤令,许志刚,等.化学试剂),2015,37(1):73.
[10]ZHU J J,RAN X Z,JIANG B Y,et al.Cereals&Oils(朱久进,冉秀芝,蒋炳英,等.粮食与油脂),2012,25(1):16.
[11]YOU G Y,CHEN B B,HE M,et al.Journal of Analytical Science(尤国颖,陈贝贝,何蔓,等.分析科学学报),2015,31(5):593.
[2]Rezanka P,NavrtilovK,Rezanka M,et al.Electrophoresis,2014,35(19):2701.
[3]SHEN H M,JI H B,WU H K,et al.Chinese Journal of Organic Chemistry(沈海民,纪红兵,武宏科,等.有机化学),2014,34(8):1549.
[4]Mik2ík I.Journal of Separation Science,2017,40(1):251.
[5]BAI Q.Chinese Journal of Chromatography(白泉.色谱),2015,33(11):1117.
[6]LIN Z A,PANG J L,HUANG H,et al.Chinese Journal of Chromatography(林子俺,庞纪磊,黄慧,等.色谱),2010,28(3):273.
[7]MoravcovD,Rantamki A H,Du2a F,et al.Electrophoresis,2016,37(7-8):880.
[8]Grange R L,Evans P A.Journal of the American Chemical Society,2014,136(34):11870.
[9]FENG F,TANG L,XU Z G,et al.Chemical Reagents(冯锋,汤令,许志刚,等.化学试剂),2015,37(1):73.
[10]ZHU J J,RAN X Z,JIANG B Y,et al.Cereals&Oils(朱久进,冉秀芝,蒋炳英,等.粮食与油脂),2012,25(1):16.
[11]YOU G Y,CHEN B B,HE M,et al.Journal of Analytical Science(尤国颖,陈贝贝,何蔓,等.分析科学学报),2015,31(5):593.