摘要
建立了血浆中尼可地尔浓度的PEEK管内聚合物整体柱固相微萃取与高效液相色谱在线联用检测方法。聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)整体柱材料为萃取介质。实验优化了影响萃取效率的参数,包括萃取流速、萃取体积、样品基底pH值等。血浆样品用磷酸盐溶液稀释后便可直接进行萃取分析。血浆中尼可地尔的检出限为1ng/g,在6—120ng/g的含量范围内具有良好的线性关系,相关系数r大于0.999。日内、日间的萃取分析相对标准偏差小于9%,加标回收率高于85%。
A method for the quantitative determination of nicorandil in human plasma was established by coupling polymer monolith in-polyether ether ketone tube solid-phase mieroextraetion to high-performance liquid chromatography( HPLC ). A poly( methaerylie acid- ethylene glycol dimethaerylate) monolith, synthesized inside a polyether ether ketone (PEEK) tube, was selected as the extraction medium. To obtain the optimum extraction efficiency, several parameters were investigated, including extraction flow-rate, extraction time, and pH value of sample matrix. The sample solution can be directly injected into the device for extraction after dilution with phosphate solution. Low detection limit( 1.0 ng/g) and quantification limit(3.3 ng/g) were obtained. The method showed good linearity ranging from 6 to 120 ng/g with a linear coefficient (r value) above 0. 999. Excellent reproducibility of the method was achieved with intra-day and inter-day preeisions(RSD) less than 3.5% and 8.8% , respectively. Recovery was higher than 85% .
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第1期18-20,25,共4页
Journal of Instrumental Analysis
基金
教育部“新世纪优秀人才支持计划”基金资助项目(NCET-05-0616)
国家杰出青年科学基金资助项目(20625516)