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目的建立血浆样品中河豚毒素(TTX)的气相色谱-质谱分析方法。方法采用3%乙酸甲醇溶液提取,Oasis MCX固相柱净化,样品液中加入3 mol/L KOH溶液和甲醇、DMF将河豚毒素转化成C9碱,经Oasis HLB固相萃取柱净化、再用硅烷化衍生剂(BSTFA+TMCS)衍生,用气相色谱-质谱联用法进行定性定量分析鉴定。结果方法定性的特征离子为m/z318、m/z376、m/z392、m/z407,定量离子为m/z392;定量测定的线性范围在5 ng/ml~200 ng/ml,相关系数在0.9998,检出限为1.0 ng/ml,定量限为5.0 ng/ml,血浆样品加标回收率为82.2%~94.7%,相对标准偏差为7.6%~8.8%。结论建立的分析方法快速、准确、选择性好,可适用于公共卫生突发事件的应急检测和临床中毒病人的诊断确证。
Objective To establish a gas chromatography-mass spectrometry method for the determination of tetrodotoxin (TTX) in plasma samples. The method was extracted with 3% acetic acid in methanol and cleaned up with Oasis MCX solid phase column. The sample solution was mixed with 3 mol / L KOH solution and methanol. The tetrodotoxin was converted to C9 base by DMF and purified by Oasis HLB solid phase extraction column. Derivatives (BSTFA + TMCS) derived by gas chromatography - mass spectrometry qualitative and quantitative analysis identified. Results The qualitative characteristic ions were m / z318, m / z376, m / z392, m / z407 and m / z392. The linear range of quantitation was 5 ng / ml ~ 200 ng / ml with correlation coefficient of 0.9998 , The detection limit was 1.0 ng / ml, the limit of quantification was 5.0 ng / ml, the spiked recoveries of plasma samples were 82.2% -94.7% with relative standard deviations of 7.6% -8.8%. Conclusion The established analytical method is rapid, accurate and selective. It can be applied to the emergency detection of public health emergencies and the diagnosis of patients with clinical poisoning.