【摘要】 目的建立衍生化高效液相色谱-串联质谱法测定人血浆中5-羟色胺(5-HT)、肾上腺素(AD)和去甲肾上腺素(NA)质量浓度。方法采用Ultimate C18(50mm×4.6mm,5μm)色谱柱,流动相为乙腈∶水∶甲酸为95∶5∶0.05(V∶V∶V),流速为0.2mL/min,柱温为室温。检测方式为多反应离子监测,正离子模式,电喷雾离子源。血浆样品经沉淀蛋白后,在pH 10.5条件下与丹酰氯发生衍生化反应,产物经乙酸乙酯萃取浓集后进样。结果标准曲线线性范围为2.5~200ng/mL;日内精密度相对标准偏差(RSD)为1.33%~8.13%,日间RSD2.86%~7.73%,均小于9%;方法回收率95.44%~109.71%,基质效应4.86%~12.81%。结论本法简单、快速,可用于人血浆中5-HT、AD和NA质量浓度测定和研究。更多还原

【Abstract】 Objective to establish a method for the determination of 5-hydroxy tryptamine(5-HT),adrenalin(AD)and noradrenalin(NA)in human plasma using pre-column derivatization HPLC-MS/MS.Methods Derivatives of the plasma samples were produced with dansyl chloride under pH 10.5,and then extracted and enriched with ethyl acetate.The detected chemicals were separated using Ultimate C18(50 mm×4.6 mm,5μm)with acetonitrile-water-formic acid=95∶5∶0.05(V∶V∶V)at 0.2 mL/min.The HPLC-MS//MS system was operated under a multiple reaction monitoring mode(MRM)using the electrospray ionization technique in positive mode.Results Linear range of the calibration curve appeared in 250-2.5 ng/mL.The method had a less than 9%intra-and inter-assay relative standard deviation(RSD),95.44%-109.71%recoveries,and 4.86%-12.81% matrix effects.Conclusion This method is simple,accurate,and suitable for detection of 5-HT,AD and NA in human plasma.更多还原