高效液相色谱-串联质谱法测定人血浆和尿液中记忆丧失性贝毒软骨藻酸

Determination of Domoic Acid in Human Plasma and Urine by High Performance Liquid Chromatography Tandem Mass Spectrometry

建立了高效液相色谱一串联三重四极杆质谱法（HPLC-MS／MS）测定人血浆及尿液中记忆丧失性贝毒软骨藻酸。人血浆及尿液样品加入6倍体积甲醇沉淀剂，涡旋离心后，取上清液进样测定。色谱柱为ZorbaxSBC18柱（150×4．6mm，5μm），柱温30℃；流动相为乙腈-0．1％甲酸水溶液（13：87，V／V），流速为1．0mL／min。该方法检测血浆和尿液中软骨藻酸的线性范围均为1．8～115μg／L，相关系数r=0．999，检出限为0．9μg／L，定量下限为1．8μg／L。该方法具有操作方便、专属性强、灵敏度高的特点，适用于人体血浆及尿液中软骨藻酸的测定。

High performance liquid chromatography（HPLC） combined with tandem mass spectrometry （LC/MS/MS） has been developed for the determination of domoic acid in human plasma and urine. 6 times volume of methanol was added to the sample for protein precipipation; after vortex-centrifuging, the floated supernatant was injected into the HPLC-MS system. The separation was performed on a Zorbax SB C18（150×4.6 mm,5 μm）,using acetonitrile and 0.1% formic acid in water（13：87,V/V） as the mobile phase with the flowrate of 1.0 mL/min. It was found that linear ranges in both plasma and urine samples were 1.8-115μg/L with the correlation coefficients of 0. 999. The limit of detection（LOD） was 0.9 μg/L and the limit of quantitation （LOQ） was 1.8 μg/L. The method is simple, selective and sensitive for detection of domoic acid in human plasma and urine.