CAJ | 학술논문

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.
채용모세관전영법화고효액상색보법직접탁분2,2′-이간기-1,1′-련이내-3,3′-이갑산(HBNC)대영체.이사충불동적β-배호정위수성첨가제,고찰배호정적충류여농도、완충액pH치급농도、분리전압、온도등인소대HBNC분리적영향.결과표명:채용10 mmol/L광정기미-β-배호정+20 mmol/L린산염완충액(pH=7.0),20 kV분리전압,HBNC대영체재20 min내체도기선분리,분리도체도3.31.채용(S)-숙-량안산기-(S)-1-(α-내기)을알수성주,정기완-을순-삼불을산(97∶3∶0.2,V/V)류동상,HBNC대영체재40 min내야기본체도기선분리.
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 of 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.