Zorpas Kostas M, Valsami Georgia N, Vryonis Evangelos V, Skoutelis Athanasios T, Archontaki Helen A
University of Athens, Department of Chemistry, Laboratory of Analytical Chemistry, 15771 Athens, Greece.
J AOAC Int. 2011 May-Jun;94(3):847-56.
An isocratic HPLC method with detection at 248 nm was developed and fully validated for the determination of tigecycline in rabbit plasma. Minocycline was used as an internal standard. A Hypersil BDS RP-C18 column (250 x 4.6 mm, 5 microm particle size) was used with the mobile phase phosphate buffer (pH 7.10, 0.070 M)-acetonitrile (76 + 24, v/v) at a flow rate of 1.0 mL/min. The elution time of tigecycline and minocycline was approximately 8.1 and 9.9 min, respectively. Calibration curves of tigecycline were linear in the concentration range of 0.021-3.15 microg/mL in plasma. The LOD and LOQ in plasma were estimated as 7 and 21 ng/mL, respectively. The intraday and interday precision values of the method were in the range of 5.0-7.1 and 5.6-9.1%, while the corresponding accuracy values were in the ranges of 92.8-111.1 and 97.6-102.3%, respectively. At the LOQ, the intraday precision was 18.7%, while intraday and interday accuracy values were 97.3 and 98.0%, respectively. Robustness of the proposed method was studied using a Plackett-Burman experimental design. A pharmacokinetic profile is presented for confirmation of the applicability of the method to pharmacokinetic studies.
建立了一种在248 nm波长处检测的等度高效液相色谱法，并对其进行了全面验证，用于测定兔血浆中的替加环素。米诺环素用作内标。使用Hypersil BDS RP-C18柱（250×4.6 mm，5μm粒径），流动相为磷酸盐缓冲液（pH 7.10，0.070 M）-乙腈（76 + 24，v/v），流速为1.0 mL/min。替加环素和米诺环素的洗脱时间分别约为8.1和9.9分钟。替加环素在血浆中0.021 - 3.15μg/mL浓度范围内的校准曲线呈线性。血浆中的检测限和定量限分别估计为7和21 ng/mL。该方法的日内和日间精密度值分别在5.0 - 7.1%和5.6 - 9.1%范围内，而相应的准确度值分别在92.8 - 111.1%和97.6 - 102.3%范围内。在定量限处，日内精密度为18.
