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目的建立并优化一种简单、快速、高该该和高选择性高效液相色谱法(HPLC)测定重症监护(ICU)患者接受连续性血液净化时(CBP)头孢吡肟的血药浓度。方法头孢他啶为内标,血浆样品用30%高氯酸沉淀蛋白后用氯仿反萃取,离心,取上层水相直接进样。样品分离用ZORBAX SB-C18柱(4.6mm×150mm,5?μm)和填充相同材料的预柱(4.6mm×12.5mm,5μm),流动相为乙腈-0.03mol·L-1醋酸铵(用醋酸调pH至4.0)(6∶94),流速1.0mL·min-1,进样体积为25μL。紫外检测波长254nm。结果头孢吡肟的血浆浓度线性范围是1～200mg·L-1,相关系数r为0.9999;低、中、高血浆质控样品,内RSD均小于3%,,间RSD均小于7%,方法平均回收率分别为115%,98.0%和97.0%。结论对比已报道的头孢吡肟血药浓度测定方法,本实验优化的方法不仅血浆样品处理简单,重现性高和选择性高,还提供更经济,更少污染及更好地保护色谱柱等优点。此外,实验结果表明,心血管类药物对测定无干扰,因此该方法更适于ICU患者接受CBP治疗时头孢吡肟的临床药动学研究。
Objective To establish and optimize a simple, rapid, high and high selective HPLC method for the determination of cefepime in patients receiving intensive blood purification (CBP) in intensive care unit (ICU). Methods Ceftazidime was used as an internal standard. After the plasma samples were precipitated with 30% perchloric acid, the samples were back-extracted with chloroform, centrifuged, and the upper aqueous phase was directly injected. The sample was separated on a ZORBAX SB-C18 column (4.6 mm × 150 mm, 5 μm) and a precolumn (4.6 mm × 12.5 mm, 5 μm) filled with the same material. The mobile phase was acetonitrile-0.03 mol·L-1 ammonium acetate Acetic acid adjusted to pH 4.0) (6:94), flow rate 1.0mL · min-1, injection volume of 25μL. UV detection wavelength 254nm. Results The linear range of cefepime was 1 ~ 200 mg · L-1 with a correlation coefficient r of 0.9999. The RSDs of all samples were less than 3%, and the RSDs were less than 7% The average recoveries were 115%, 98.0% and 97.0%, respectively. Conclusion Compared with the reported method for determination of cefepime in plasma, the optimized method in this experiment not only has the advantages of simple, high reproducibility and high selectivity of plasma samples, but also provides more economical, less pollution and better protection of chromatography columns advantage. In addition, the experimental results show that the cardiovascular drugs do not interfere with the determination, so the method is more suitable for clinical pharmacokinetics of cefepime when ICU patients receive CBP.