摘要
研究了反相高效液相色谱测定双氯灭痛血药浓度的新方法，考察了蛋白沉淀剂乙腈用量、流动相ｐＨ值等对血药色谱行为的影响。优化的色谱条件为：Ｃ（１８）Ｈｙｐｅｒｓｉｌ（５μｍ，１００ｍｍ×４．６ｍｍ）不锈钢柱，甲醇－乙腈－ｐＨ６．０磷酸盐缓冲液（２５：２０：５５）作流动相，检测波长２８０ｎｍ，进样量５０μｌ。采用乙腈沉淀蛋白后直接进样，操作简便快速，回收率达９９．１８％～１０３．６％，日内ＲＳＤ为３．４％～３．７％，日间ＲＳＤ４．４％～４．９％，血药浓度在０．２５～８．Ｏμｇ／ｍｌ线性关系良好，ｒ＝０．９９９４，血药最低检测浓度为２００ｎｇ／ｍｌ。
A sensitive and selective RP-HPLC procedure has been developed to determine diclofenac in human serum.A 100 mm× 4.6 mm C(18)Hypersil(5 μm)column with a mobile phase consisting of metanol-acetonitrile-pH6.0 phosphate buffer(25:20:55)was used.Effect of the proportion of protein precipitant acetonitrile and the pH of mobile phase on the peak shape of diclofenac in serum was studied.The serum sample was deproteinized by adding acetonitrile and a 50 μl portion of the supernatant after centrifugation was directly chromatographed.Standard curve was linear over the concentration range of 0.25～8.0μg/ml and the detective limit in serum was 200 ng/ml using ultraviolet detection at 280 nm.The proposed method was simple and accurate,and the recoveries were 99.18%～103.6%% with the within-day RSD from 3.4%～3.7% and the between-day RSD from 4.4%～4.9%.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
1995年第1期23-26,共4页
Journal of China Pharmaceutical University
