毛细管电泳法和高效液相色谱法拆分联萘二酚酸对映体  

Enantioseparation of 2,2′-Dihydroxy-1,1′-dinaphthyl-3,3′-dicarboxylic Acid by Capillary Electrophoresis and High-performance Liquid Chromatography

作　　者：徐小静[1] 王丽莉[2] 阮源萍[1] 

机构地区：[1]厦门大学现代分析科学教育部重点实验室,福建厦门361005 [2]厦门大学化学化工学院,福建厦门361005

出　　处：《分析科学学报》2009年第5期547-550,共4页Journal of Analytical Science

基　　金：国家自然科学基金(No.20572088);福建省自然科学基金(No.C0510001)

摘　　要：采用毛细管电泳法和高效液相色谱法直接拆分2,2′-二羟基-1,1′-联二萘-3,3′-二甲酸(HBNC)对映体。以四种不同的β-环糊精为手性添加剂,考察环糊精的种类与浓度、缓冲液pH值及浓度、分离电压、温度等因素对HBNC分离的影响。结果表明:采用10 mmol/L磺丁基醚-β-环糊精+20 mmol/L磷酸盐缓冲液(pH=7.0),20 kV分离电压,HBNC对映体在20 min内达到基线分离,分离度达到3.31。采用(S)-叔-亮氨酸基-(S)-1-(α-萘基)乙胺手性柱,正己烷-乙醇-三氟乙酸(97∶3∶0.2,V/V)流动相,HBNC对映体在40 min内也基本达到基线分离。Enantioseparation of 2,2′-dihydroxy-1,1′-dinaphthyl-3,3′-dicarboxylic acid（HBNC） has been investigated by CZE and HPLC.Neutral β-cycledextrin（β-CD）,methyl-β-cycledextrin（Me-β-CD） and hydroxypropyl-β-cycledextrin（HP-β-CD）,as well as negative sulfobutyl ether β-cycledextrin（SBE-β-CD） were applied as chiral selectors,and were evaluated for enantioseparation of HBNC by CZE.The parameters,such as the kind of β-CD selector,concentration of SBE-β-CD,pH and concentration of buffer,applied voltage,have been studied in detail. Under the optimum conditions：10 mmol/L SBE-β-CD with 20 mmol/L phosphate （pH = 7.0） as a running buffer, applied voltage ot 20 kV, capillary temperature at 25℃, and detection at 229 nm, baseline separation of HBNC enantiomers could be achieved within 20 mins by CZE. Furthermore, a better separation of HBNC enantiomers was obtained on the CHIREX （S）-LEU ＆ （S）-NEA column with n-hexane/ethanol/ trifluoacetic acid （97：3：0.2 by volume） as mobile phase within 40 mins by HPLC.

关 键 词：对映体拆分 毛细管区带电泳 高效液相色谱 磺丁基醚-Β-环糊精 

分 类 号：O657.8[理学—分析化学]