建立了液相色谱-质谱法测定织纹螺中河豚毒素的分析方法.匀质后的样品用0.03 mol/L乙酸溶液提取,水浴加热10 min,用Sep-Pak C18固相萃取柱净化,再用截留相对分子质量为3 000的超滤管过滤.采用Insertsil ODS-3色谱柱分离,以含有30 mmol/L七氟丁酸的甲酸铵溶液(1 mmol/L)-甲醇(体积比为99∶1)为流动相,采用电喷雾离子源,选择离子监测模式检测.以保留时间和河豚毒素的二级质谱特征碎片离子予以定性确证.结果表明,在此分析条件下,可将河豚毒素及其衍生物分离,在0.01～10.0 mg/L范围内线性关系良好(r2＞0.995),检出限(以3倍信噪比为计)为2 μg/L,平均加标回收率为72.5%～80.4%,相对标准偏差为4.48%～8.87%.将该方法用于实际样品检测,在赤潮后所采集的织纹螺样品中检出了河豚毒素.
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