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目的建立测定人血浆中头孢泊肟酯的活性代谢产物头孢泊肟浓度的高效液相色谱法,并应用于头孢泊肟酯干混悬剂在健康人体内的药动学研究。方法采用沉淀蛋白法进行样品预处理,色谱柱为Agilent Zorbax SB-C18柱(150 mm×4.6 mm,5μm),流动相为乙腈-20 mmol.L-1磷酸二氢铵缓冲液(体积比为9∶91,含6.6 mmol.L-1三乙胺,磷酸调pH值至2.0),流速为1.0 mL.min-1,检测波长为254 nm,内标为头孢克洛。结果头孢泊肟浓度线性范围为0.102～6.528 mg.L-1,低、中、高3个质量浓度的提取回收率分别为92.0%、93.3%和92.1%,日内和日间精密度RSD(n=6)分别为3.3%、3.8%、2.0%和14.2%、2.9%、6.3%。头孢泊肟血浆样品室温放置2 h、预处理后室温放置24 h、经历1次及3次冷冻-解冻循环和-20℃冷冻情况下保存40 d均可保持稳定。结论此法适用于头孢泊肟酯药动学研究。
Objective To establish a HPLC method for the determination of cefpodoxime, the active metabolite of cefpodoxime proxetil in human plasma, and to study the pharmacokinetics of cefpodoxime proxetil suspension in healthy volunteers. Methods Precipitation protein was used for sample pretreatment. The column was Agilent Zorbax SB-C18 column (150 mm × 4.6 mm, 5 μm) and the mobile phase consisted of acetonitrile-20 mmol.L-1 ammonium dihydrogen phosphate buffer (volume ratio 9:91, containing 6.6 mmol.L-1 triethylamine, adjusted to pH 2.0 with phosphoric acid) at a flow rate of 1.0 mL.min-1 at a detection wavelength of 254 nm with an internal standard of cefaclor. Results The linear range of cefpodoxime was 0.102 ~ 6.528 mg.L-1. The recoveries of three concentrations of low, medium and high concentration were 92.0%, 93.3% and 92.1%, respectively. The intra- and inter-day precision RSD (n = 6) were 3.3%, 3.8%, 2.0% and 14.2%, 2.9% and 6.3% respectively. Cefpodoxime plasma samples were stored at room temperature for 2 h and pretreated for 24 h at room temperature. The samples were stable after 1 and 3 freeze-thaw cycles and at -20 ℃ for 40 days. Conclusion This method is suitable for cefpodoxime ester pharmacokinetic studies.