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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。
Objective To establish a highly sensitive method for the detection of tetrodotoxin, a small molecule biotoxin in biomedical samples. A new LC - TOF mass spectrometry method was developed for the detection of tetrodotoxin in human plasma. The optimal conditions of liquid chromatography - tandem mass spectrometry Mass spectrometry conditions, investigated the method of extracting tetrodotoxin in plasma. Results For the reference solution, the linear range of tetrodotoxin was 0.1-50 mg / L and the limit of detection was 0.01 mg / L. The linear range of tetrodotoxin was 0.5-10 mg / L and the detection limit was 0.25 mg / L. Conclusion The established liquid chromatography-time of flight mass spectrometry method is of high specificity and high sensitivity and can be applied to the actual detection of tetrodotoxin at mg / L in puffer fish head samples.