在线固相萃取-高效液相色谱法测定人血清中左旋舒必利

Determination of Levosulpiride in Human Serum by On-line Solid Phase Extraction-High Performance Liquid Chromatography

建立了分析人血清样品中左旋舒必利(Levosulpiride)含量的在线固相萃取-高效液相色谱法。人血清样品用甲醇简单沉淀蛋白处理后,直接进样分析。首先通过固相萃取泵将样品载入到CAPCELLPAKSCX UG80固相萃取柱(10×4.0 mm)进行富集净化,然后通过阀切换将固相萃取柱切换至分析流路中,分析泵将保留在固相萃取柱上的目标物冲洗至Acclaim Mixed-Mode WCX-1分析柱(150×3.0 mm,3μm)进行分离,二极管阵列检测器检测。结果表明:人血清中左旋舒必利在50~1 600 ng/mL质量浓度范围内线性良好,线性相关系数r=0.9997,检出限为3.5 ng/mL,低、中、高3个浓度水平的加标回收率为85.0%~102.9%,其日内和日间相对标准偏差均小于7.2%。该方法专属性强,灵敏度高,重复性好,经济适用,适用于人血清中左旋舒必利浓度的测定,可用于血清中左旋舒必利的临床血药浓度检测及药代动力学研究。

A rapid,simple and accurate on-line solid phase extraction(On-line SPE)-HPLC method for the detection of Levosulpiride in human serum was established.Human serum samples were treated with simple protein precipitation using methanol and directly injected for analysis.Firstly,sample was injected into the CAPCELLPAKSCX UG80(10×4.0 mm)(Shiseido)cartridge for on-line SPE and purification,then the cartridge was switched to the analytical system by valve switching.The Levosulpiride retained on the SPE column was flushed into the Acclaim Mixed-Mode WCX-1(150×3.0 mm,3μm)analytical column for separation and was detected by a diode array detector.The Levosulpiride showed good linearity between 50 ng/mL and 1 600 ng/mL,with the detection limit of 3.5 ng/mL.The serum spiked recoveries of Levosulpiride were between 85.0%and 102.9%.The intra-day and inter-day stability were also studied with relative standard deviations of less than 7.2%.This method would be useful for the clinical monitoring and pharmacokinetic study of levosulpiride in serum.