摘要
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 。
Aim To establish separation methods of five sulfonamides by using capillary high performance liquid chromatography(μ HPLC) and electrochromatography. The effect of mobile phase varies such as methanol content, pH, buffer solution concentration and voltage on their chromatographic behavior and electroosmesis flow was investigated. Capillary electrochromatography(CEC) was compared with μ HPLC at the same condition.Methods Stationary phase was ODS, mobile phase was methanol and 2 mmol·L -1 H 3PO 4 buffer solution (pH 3 0-7 0), voltage was 0- -15 kV, flow rate was 10 μL·min -1 , pressure was approximately 70 MPa and UV detection wavelength was 254 nm. Results Separations on base line have been respectively accomplished for five sulfonamides by μ HPLC with mobile phase of methanol 2 mmol·L -1 H 3PO 4 buffer solution (30∶70) at pH 5 0 in 67 min, and CEC with the same mobile phase at -5 kV voltage in 25 min. Conclusion Electroosmesis flow of CEC decreased with the increase in methanol content, buffer solution concentration, increased with the increase in voltage and increase slightly with the increase in pH of mobile phase. Retention values ( k ) of solutes to be examined decreased with increasing methanol content of mobile phase in μ HPLC and CEC. Retention values ( k ) of solutes increased slightly with increasing buffer solution concentration, decreased with increasing voltage in CEC. Trimethoprim(TMP) decreased obviously with increasing voltage in CEC. The effect of pH of mobile phase on retention values ( k ) was more complex. Five sulfonamides were separated at the same mobile phase condition by μ HPLC and CEC. And separation speed of CEC was much faster than that of μ HPLC. CEC was very fit for rapid separation of sulfonamides.
出处
《药学学报》
CAS
CSCD
北大核心
2003年第2期129-132,共4页
Acta Pharmaceutica Sinica
关键词
磺胺类药物
毛细管高效液相色谱
电色谱
sulfacetamide sodium
sulfadiazine
sulphadimidine
sulphamethoxazole
trimethoprim
capillary high performance liquid chromatography
capillary electrochromatography
