摘要
目的 :开发一个可用于定量测定胆汁中头孢美唑 (又称先锋美他醇 )浓度的高效液相色谱分析方法。方法 :取 0 2mL胆汁用水稀释至 1mL ,并转移至已准备好的C18固相萃取柱中进行固相萃取。用 1mL 10 %乙腈水溶液洗脱吸附在固相萃取柱上的头孢美唑 ,并收集于样品瓶中 ,用高效液相色谱法进行分析测定。流动相为 2 0∶80的乙腈∶缓冲溶液 (0 0 1moL/L磷酸盐 ,0 0 1%TBA ,pH7 0 )。检测波长为 2 72nm。结果 :本分析方法在 (1 2 5~ 2 5 ) μg/mL的浓度范围内呈良好线性 (γ =0 9999) ;方法回收率在 88 0 %~ 10 3 %之间 ,日内与日间相对标准偏差 <5 2 % ;方法的检测下限与定量下限分别为 1 2 μg/mLand2 4μg/mL。
Objective:To develop an analytical method for the quantitative determination of cefmetazole in bile.Method:An aliquot of 0 2 mL bile was diluted to 1 mL with deionized water and applied onto a preconditioned C18 solid phase extraction cartridge.Cefmetazole was eluted from the cartridge with 1 mL of 10% acetonitrile in water and then analyzed with ion-paired reverse phase high performance liquid chromatography with uv detection.Mobile phase was 20∶80 acetonitrile∶buffer (0 01moL/L phosphate with 0 01%TBA,pH 7 0).The wavelength of the detector was set at 272nm.Results:The analytical method gave good linearity in the concentration range of (1 25~25) g/mL of cefmetazole in bile(γ=0 9999).The method recoveries at different concentration levels were between 88 0%~103% with within-day and day to day relative standard deviations less than 5 2%.The method detection limit and quantitation limit were 1 2 g/mL and 2 4μg/mL of cefmetazole in bile,respectively.
出处
《汕头大学医学院学报》
2000年第2期4-6,共3页
Journal of Shantou University Medical College