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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 a HPLC method for the quantitative determination of cefmetazole (avant-garde memantine) in bile. METHODS: 0 2 mL bile was diluted to 1 mL with water and transferred to a prepared C18 solid-phase extraction cartridge for solid-phase extraction. Cefmetazole adsorbed onto the SPE column was eluted with 1 mL of 10% acetonitrile in water and collected in a vial for analysis by high performance liquid chromatography. Acetonitrile with a mobile phase of 20:80: buffer solution (0.01 mol / L phosphate, 0.01% TBA, pH 7.0). Detection wavelength of 722nm. Results: The method showed a good linearity (γ = 0 9999) in the range of (1 2 5 ~ 2 5) μg / mL. The recoveries were between 88 0% and 103% The standard deviation was <52%. The lower limit of detection and the lower limit of quantitation were 12 μg / mL and 24 μg / mL, respectively.