建立了一种采用中空纤维离心超滤(HFCF-UF)-高效凝胶排阻色谱法(HPSEC)对青霉素V钾中的残留蛋白进行检测的方法。样品用HFCF-UF进行富集,采用HPSEC进行分析,色谱柱为TSK gel Super SW2000凝胶色谱柱(300×4.6mm,4μm),流动相为0.06m...建立了一种采用中空纤维离心超滤(HFCF-UF)-高效凝胶排阻色谱法(HPSEC)对青霉素V钾中的残留蛋白进行检测的方法。样品用HFCF-UF进行富集,采用HPSEC进行分析,色谱柱为TSK gel Super SW2000凝胶色谱柱(300×4.6mm,4μm),流动相为0.06mol/L NaCl-0.02mol/L NaH_2PO_4(pH=7.0),流速为0.3mL/min,紫外检测波长为220nm,柱温为室温。对照品牛血清白蛋白(BSA)在1.0~100.0μg/mL内线性关系良好(R2=0.999),回收率均大于87%,检测限为3.03ng/mL,经HFCF-UF富集处理后,富集倍数(EF)高达99倍。结果表明,该方法操作简便、结果准确、灵敏度高,为同类药物中的大分子蛋白检测提供了有效手段。展开更多
The purpose of this study was to establish a method for determining the free concentration of ceftriaxone based on hollow fiber centrifugal ultrafiltration(HFCF-UF)technology in combination with high-performance liqui...The purpose of this study was to establish a method for determining the free concentration of ceftriaxone based on hollow fiber centrifugal ultrafiltration(HFCF-UF)technology in combination with high-performance liquid chromatography(HPLC)for free pharmacokinetic studies and the prediction of ceftriaxone concentrations in lung tissue.This method only required centrifugation for a short time,and the filtrate could be injected directly for HPLC analysis without further treatment.The specificity,linearity,precision and stability of this method were validated for quantification of free ceftriaxone.Under the optimized conditions,the absolute recoveries were more than 92.5%.The intraday and interday precision RSDs were less than 3.6%.Additionally,nonspecific adsorption(NSB)between the analyte and the ultrafiltration membrane was considered.This method was successfully applied to the analysis of the free ceftriaxone concentration in rat plasma and lung tissue.The free ceftriaxone concentration of lung tissue could be predicted by using the linear formula Cfl=Cfp(0.342 x–0.0129)(x:time).This method also provides a reliable alternative for accurate monitoring of the free ceftriaxone concentration in therapeutic drug monitoring(TDM).展开更多
文摘建立了一种采用中空纤维离心超滤(HFCF-UF)-高效凝胶排阻色谱法(HPSEC)对青霉素V钾中的残留蛋白进行检测的方法。样品用HFCF-UF进行富集,采用HPSEC进行分析,色谱柱为TSK gel Super SW2000凝胶色谱柱(300×4.6mm,4μm),流动相为0.06mol/L NaCl-0.02mol/L NaH_2PO_4(pH=7.0),流速为0.3mL/min,紫外检测波长为220nm,柱温为室温。对照品牛血清白蛋白(BSA)在1.0~100.0μg/mL内线性关系良好(R2=0.999),回收率均大于87%,检测限为3.03ng/mL,经HFCF-UF富集处理后,富集倍数(EF)高达99倍。结果表明,该方法操作简便、结果准确、灵敏度高,为同类药物中的大分子蛋白检测提供了有效手段。
文摘The purpose of this study was to establish a method for determining the free concentration of ceftriaxone based on hollow fiber centrifugal ultrafiltration(HFCF-UF)technology in combination with high-performance liquid chromatography(HPLC)for free pharmacokinetic studies and the prediction of ceftriaxone concentrations in lung tissue.This method only required centrifugation for a short time,and the filtrate could be injected directly for HPLC analysis without further treatment.The specificity,linearity,precision and stability of this method were validated for quantification of free ceftriaxone.Under the optimized conditions,the absolute recoveries were more than 92.5%.The intraday and interday precision RSDs were less than 3.6%.Additionally,nonspecific adsorption(NSB)between the analyte and the ultrafiltration membrane was considered.This method was successfully applied to the analysis of the free ceftriaxone concentration in rat plasma and lung tissue.The free ceftriaxone concentration of lung tissue could be predicted by using the linear formula Cfl=Cfp(0.342 x–0.0129)(x:time).This method also provides a reliable alternative for accurate monitoring of the free ceftriaxone concentration in therapeutic drug monitoring(TDM).
