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目的 研究毛细管高效液相色谱 ( μ HPLC)和毛细管电色谱 (CEC)分离磺胺类药物 ,建立药物微分离分析方法。方法 用ODS柱为固定相 ,甲醇和 2mmol·L- 1 磷酸缓冲液 (pH 3 0~ 7 0 )为流动相 ,电压为 0~ - 15kV ,流速为 10 μL·min- 1 ,紫外检测波长 2 5 4nm。结果 μ HPLC在甲醇 2mmol·L- 1 磷酸缓冲液 ( 3 0∶70 ) ,pH 3 0时 5种磺胺类药物实现基线分离 ;CEC在电压为 - 5kV ,甲醇 2mmol·L- 1 磷酸缓冲液 ( 3 0∶70 ) ,pH 5 0时 5种磺胺类药物实现基线分离。结论 电渗流随甲醇含量、缓冲液浓度增加而下降 ,随pH值、电压的增加而增加 ;溶质的保留值 (k)随甲醇含量、缓冲液浓度、电压的增加而下降 ,随电压增加下降明显的是TMP ,随pH值变化较复杂。在相同条件下对 5种磺胺类药物的分离 ,μ HPLC需 67min ,CEC只需 2 5min ,后者更适合于磺胺类药物的快速分离分析
Objective To study the separation of sulfonamides by capillary high performance liquid chromatography (HPLC) and capillary electrochromatography (CEC), and to establish a method of micro-separation of drugs. Methods ODS column was used as the stationary phase. Methanol and 2 mmol·L-1 phosphate buffer (pH 30 ~ 70) were used as the mobile phase at a voltage of 0 ~ -15 kV with a flow rate of 10 μL · min-1. The UV detection wavelength was 2 5 4nm. Results μ HPLC separation of 5 sulfonamides in methanol 2mmol·L-1 phosphate buffer (30:70) and pH 3 was achieved. CEC was separated at a voltage of-5kV in methanol 2mmol·L-1 phosphate buffer 3 0:70). Five sulfonamides were baseline-separated at pH 5.0. CONCLUSION: The electroosmotic flow decreases with the increase of methanol concentration and buffer concentration, and increases with the increase of pH and voltage. The retention (k) of solute decreases with the increase of methanol concentration, buffer concentration and voltage, and decreases with increasing voltage The TMP, with the pH changes more complicated. Under the same conditions for the separation of five sulfonamides, μ HPLC 67min, CEC only 25min, which is more suitable for the rapid separation of sulfonamides