Objective To establish a highly sensitive method suitable for detection of intoxicated biomedical samples with regard to tetrodotoxin ,one of the most toxic non-proteins as well as a hydrophilic small biotoxin . Methods A novel method for detection of tetrodotoxin in human blood plasma by liquid chromatography -time of flight/mass spectrometry ( LC-TOF/MS) technique was established using a cation exchange -reverse phase separation mode. The LC-MS analysis and extraction conditions were systematically optimized. Results For the tetrodotoxin standard sample , the linear calibration curve ranged from 0.1 to 50 mg/L and the limit of detection ( LOD) was 0.01 mg/L. For the tetrodotoxin exposed human plasma sample, the linear calibration curve ranged from 0.5 to 10 mg/L and the LOD was 0.25 mg/L, respectively. Conclusion Such an LC-TOF/MS established for the detection of tetrodotoxin is highly specific and sensitive , and it can be feasible for the detection of tetrodotoxin at mg/L level in puffer fish biosamples.%目的 建立一种可用于检测中毒生物医学样品中小分子生物毒素--河豚毒素的高灵敏度分析方法.方法 选用阳离子交换-反相混合色谱柱,针对河豚毒素亲水性强的特点,建立了一种新型的液相色谱-飞行时间质谱方法对人血浆中河豚毒素进行检测,优化了液相色谱-质谱条件,考察了血浆中河豚毒素的提取方法.结果 对于参考品溶液,河豚毒素的线性范围为0.1～50 mg/L,检测限为0.01 mg/L;对于染毒人血浆样品,河豚毒素的线性范围为0.5～10 mg/L,检测限为0.25 mg/L.结论 所建立的液相色谱-飞行时间质谱方法专属性强、灵敏度高,可适用于实际测定河豚鱼头样品中 mg/L水平的河豚毒素.
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