Clinical Pharmacology Unit, Department of Clinical Biochemistry, Institute of Cardiology, Alpejska 42, 04-628 Warsaw, Poland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Dec 12;911:133-9. doi: 10.1016/j.jchromb.2012.11.002. Epub 2012 Nov 12.
The paper presents an HPLC method for cefazolin determination in human serum. The preparation step was based on serum protein precipitation with acetonitrile followed by supernatant evaporation and sample reconstitution in water before injection. The separation of cefazolin and internal standard cefamandole was performed at ambient temperature under isocratic conditions on LiChrosorb RP8-5 column (250mm×4.6mm) using the mixture: CH(3)CN:H(2)O:0.5M KH(2)PO(4) (100:894:6, v/v) as a mobile phase with a flow rate of 1.5mL/min. UV detection was performed at 272nm with LLOQ of 0.2μg/mL. The precision was satisfactory in the whole range tested with RSD of 2.3-12.5% (accuracy: from -2.3% to +3.6%) and of 1.7-7.1% (accuracy: from -3.5% to +1.1%) for intra- and inter-assay, respectively. The method stability was confirmed in a series of experiments including: freeze-thaw and short- and long-term stability testing. Finally, the procedure described was found resistant to potential human errors.
本文介绍了一种用于人血清中头孢唑林测定的 HPLC 方法。该方法的制备步骤基于用乙腈沉淀血清蛋白，然后将上清液蒸发，再用水重新溶解进样。头孢唑林和内标头孢孟多的分离是在室温下，等度条件下，在 LiChrosorb RP8-5 柱（250mm×4.6mm）上进行的，流动相为 CH(3)CN:H(2)O:0.5M KH(2)PO(4)（100:894:6，v/v），流速为 1.5mL/min。UV 检测波长为 272nm，LLOQ 为 0.2μg/mL。该方法在整个测试范围内的精密度均令人满意，日内和日间精密度的 RSD 分别为 2.3-12.5%（准确度：-2.3%至+3.6%）和 1.7-7.1%（准确度：-3.5%至+1.1%）。该方法在一系列实验中稳定性得到了验证，包括：冻融和短期及长期稳定性测试。最后，发现所描述的程序能够抵抗潜在的人为错误。
