血浆中双氯芬酸钾含量测定方法学研究

STUDY ON ASSAY OF DICLOFENAC POTASSIUM IN HUMAN PLASMA

目的 :为了测定血浆双氯芬酸钾特建立反相高效液相色谱测定法。方法 :反相高效液相色谱法。色谱柱 :HypcrsilODSC18柱 ,5μm( 2 50× 4 .6)mmI .D ;流动相 :甲醇— 2 0mmol/L磷酸二氢钾液 ,用磷酸调至 pH 2 .5;流速 :1ml/min ;柱温 :4 3℃ ;检测波长 :2 82nm。结果 :线性方程为As/Ai=2 .881× 1 0 -3C -0 .0 0 2 1 ,r =0 .9998,线性范围为 ( 1 6～ 1 2 80 0 ) μg/L ,高、中、低三种浓度的双氯芬酸钾测得的日内精密度小于 2 .99% ,日间精密度小于 6.67% ,平均回收率为 ( 99.58± 1 .0 9) %。血浆最低检测浓度为 5μg/L。 结论 :该方法简便、准确、稳定 ,可用于测定血浆双氯芬酸钾浓度和该药药代动力学研究。

Objective:To establish a method for assay of diclofenac potassium in human plasma.Methods:A liquid liquid extraction method was used.This method involved a C 18 column as stationary phase and phosphate buffer methanol(65:35) as mobile phase.Detection wavelength was 282nm.The speed of flow was 1.2ml/min.Results:The limit of detection was 5μg/L.The calibration curve was linear between (16～12800) μg/L with a regression coefficient 0.9998.Interday RSD was less than 2.99% and intra day RSD was less than 6.67%.The mean recovery was (99.58+1.09)%(n=15).Conclusion:This method can be applied to study pharmacokinetics and bioavailability of diclofenac potassium. ( J Hangzhou Med Coll,2000,21:181～182 )