1-萘基-3-甲基-5-吡唑啉酮衍生单糖胶束电动毛细管色谱分离条件考察  

Investigation on separation conditions of NMP-derivatized carbohydrates by micellar electrokinetic capillary

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作  者:盛筱[1] 高桂花[1] 王云龙[1] 魏开芳[1] 

机构地区:[1]济宁医学院药学院,山东日照276826

出  处:《济宁医学院学报》2010年第4期229-231,共3页Journal of Jining Medical University

摘  要:目的以1-萘基-3-甲基-5-吡唑啉酮(NMP)作为柱前衍生试剂,采用胶束电动毛细管色谱模式考察并优化糖类衍生物的分离条件。方法实验采用58.5cm×50μmi.d.毛细管(有效柱长50cm),分别考察缓冲溶液浓度、pH值、表面活性剂浓度、温度、电压及添加剂对分离的影响。结果最终在27mmol/L硼酸盐缓冲溶液(pH9.01),十二烷基硫酸钠(SDS)浓度30mmol/L,20℃,24kV,10s进样,254nm二极管阵列检测(DAD),不加任何添加剂的情况下实现了8种单糖的基线分离,结果令人满意。结论缓冲溶液浓度、pH值和表面活性剂对分离影响较大,而温度、电压和添加剂影响相对较小。Objective To investigate and optimize the separation conditions of derivatized carbohydrates using 1-naphthyl-3-methyl-5-pyrazolone(NMP)as derivatization reagent by micellar electrokinetic capillary chromatog-raphy.Methods The influence of buffer concentration,pH value,concentration of surfactant,temperature,voltage,and other additives on separation conditions were investigated respectively at a 58.5 cm×50μm i.d.(50 cm effective length)untreated fused-silica capillary.Results 8 NMP-derivatized carbohydrates achieved baseline resolution at the condition of 27 mmol/L borate buffer(pH9.01),voltage 24 kV,column temperature 20℃,injection time 10 s and DAD detection 254 nm.Conclusion Buffer concentration,pH value,and concentration of surfactant had great effects on separation,while temperature,voltage,and other additives had less.

关 键 词:单糖 1-萘基-3-甲基-5-吡唑啉酮(NMP) 胶束电动毛细管色谱 

分 类 号:O657[理学—分析化学]

 

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