摘要
建立了测定猪血浆中去呋喃甲酰基头孢噻呋(DFC)的高效液相色谱法(HPLC).血浆样品经DTE-磷酸缓冲液提取,过SPE小柱净化浓缩,甲醇洗脱,用XDB-C18色谱柱分离,流动相由乙腈(A)和0.1%三氟乙酸水溶液(B)组成.采用梯度洗脱:0 min为12%A和88%B,15 min为18%A和82%B,18 min为12%A和88%B,平衡至20 min.流速0.8 mL.min-1,波长266 nm.以DFC峰面积定量,浓度在0.25-40.0μg.mL-1时,其峰面积与浓度呈良好的线性关系,r2=0.9987,平均回收率为82.1%-87.4%,其日内和日间变异系数(RSD)分别为5.04%-8.58%和6.83%-9.34%.该方法适用于血浆中DFC的浓度测定和药代动力学研究.
High performance liquid chromatography(HPLC) was established to determine desfuroylceftiofur(DFC) in pig plasma.Plasma sample was extracted with dithioerythritol-phosphate buffer,then concentrated and purified by SPE course and eluted with methanol.Chromatographic separation was carried out on a XDB-C18 chromatographic column,the mobile phases consisted of acetonitrile(A) and 0.1% trifluoroacetic acid solution(B).A gradient elution procedure was performed: 12%A and 88%B at 0 min,18%A and 82%B at 15 min,12%A and 88%B at 18 min,then balanced to 20 min.The flow rate was 0.8 mL·min-1,the wave length of DAD detector was 266 nm.The determination was quantitated according to peak area of DFC.The calibration curve was linear in the range of 0.25-40.0 μg·mL^-12=0.9987),and the average recovery was 82.1%-87.4%,relative standard deviations(RSD) of inter-day and intra-day were 5.04%-8.58% and 6.83%-9.34%,respectively.The method could be applied to the concentration determination of DFC in plasma and pharmacokinetics research.
出处
《福建农林大学学报(自然科学版)》
CSCD
北大核心
2010年第1期58-62,共5页
Journal of Fujian Agriculture and Forestry University:Natural Science Edition