PEEK管内聚合物整体柱固相微萃取／高效液相色谱在线联用对血浆中尼可地尔的测定

Determination of Nicorandil in Human Plasma Using Polymer Monolith In-polyether Ether Ketone Tube Solid-phase Microextraction On-line Coupled to High Performance Liquid Chromatography

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% .