固相萃取法用于生物样品中头孢克肟浓度测定的样品准备

Sample preparation for chromatographic determination of cefixime in biological samples by solid-phase extraction method

目的 建立反相固相萃取法 ,用于血浆和支气管肺胞灌流液 (BAL)中头孢克肟 (CFX)浓度测定的准备 ,并以HPLC法测定CFX含量。方法 用Sep pakC18固相萃取柱富集、提取生物样品中CFX ,对固相萃取的上样速度、洗脱用缓冲液pH值、洗脱用甲醇体积对回收率的影响进行了研究 ,并选择了最佳样品处理条件。结果 CFX血浆浓度在 0 .1～ 4.0 μg/ml,BAL中浓度在 0 .0 12 5～ 0 .4μg/ml范围内具有良好线性关系 ;CFX在血浆和BAL中的回收率分别为 ( 99.2± 2 .36 ) %和 ( 97.9± 2 .77) % ;血浆及BAL样品的日内、日间RSD均小于 5 %。结论 本法简单、灵敏 ,适用于生物样品中CFX浓度的测定。

Objective To establish solid phase extraction method for plasma and bronchoalveolar lavage fluid (BAL) sample preparation and determination of cefixime with RP HPLC. Methods Cefixime in biological fluids were extracted and enriched by Sep pak C 18 solid phase columns. During extraction the flow rate of sample loading, pH value of sample solution and the volume of eluting methanol were studied for obtaining satisfactory recovery. Results The standard curves of cefixime in plasma and in BAL were linear in the range from 0.1～4.0 μg/ml ( r=0.9999)and 0.0125～0.4 μg/ml ( r =0.9998) respectively. The average recoveries were (99.2+2.36)% ( n =4) in plasma and (97.9+2.77)% ( n =4) in BAL. Conclusion This method is sensitive and simple and suitable for determining low concentration of cefixime in biological fluids.