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目的针对海产品常见中毒原因分析需求,建立基质分散固相萃取净化-亲水液相色谱-串联三重四极杆质谱(HILIC-MS/MS)快速定性定量检测织纹螺和贝类中河鲀毒素的新方法。方法 1.0 g样品经0.1%乙酸溶液沸水浴提取后,用50 mg亲水亲油平衡填料(HLB)和5 mg石墨化碳黑(GCB)吸附剂吸附净化,最后经乙腈蛋白沉淀后过0.22μm聚四氟乙烯(PTFE)滤膜,亲水液相色谱柱(150 mm×2.0 mm,3μm)分离,电喷雾离子化,选择反应监测(SRM)模式检测,基质匹配外标法定量。结果在2.0~40.0 ng/ml浓度范围内,河鲀毒素呈现良好的线性关系,相关系数r~2≥0.999;以3倍基线噪声所对应的浓度为检出限时,河鲀毒素的方法检出限可达10.0μg/kg;在25、100和200μg/kg的加标水平时,方法回收率为74.2%~87.9%,相对标准偏差为2.3%~9.1%。应用本方法对浙江沿海地区市售织纹螺和贝类样品进行检测,15份织纹螺中有14份检出河鲀毒素,检出率为93.3%,含量范围为0.04~15.75 mg/kg,60份贝类样品均未检出河鲀毒素。结论该检测方法准确、快速、易操作,能满足典型海产品中河鲀毒素的公共卫生应急检测或日常监测要求。
OBJECTIVE To rapidly analyze the causes of common poisoning in seafood and establish a matrix-dispersive SPE-HPLC-tandem mass spectrometry (HILIC-MS / MS) New method of toxins. Methods 1.0 g sample was extracted with 0.1% acetic acid solution in boiling water bath and purified by adsorption with 50 mg HLB and 5 mg GCB adsorbent. Polytetrafluoroethylene (PTFE) membrane, separation of hydrophilic liquid chromatography column (150 mm × 2.0 mm, 3 μm), electrospray ionization, selective reaction monitoring (SRM) mode and matrix matching external standard were used. Results The concentration of tetrodotoxin showed a good linear relationship in the concentration range of 2.0-40.0 ng / ml with the correlation coefficient of r ≥ 2 ≥ 0.999. When the concentration corresponding to 3-fold baseline noise was the detection limit, tetrodotoxin was detected The limit of detection was up to 10.0μg / kg. The method recoveries ranged from 74.2% to 87.9% with relative standard deviations of 2.3% -9.1% at spiked levels of 25, 100 and 200 μg / kg. This method was applied to detect snails and shellfish in the coastal area of Zhejiang Province. Totoxin was detected in 14 of 15 snails, with a detection rate of 93.3% and a range of 0.04 ~ 15.75 mg / kg , 60 samples of shellfish were not detected tetrodotoxin. Conclusion The detection method is accurate, rapid and easy to operate, and can meet the public health emergency detection or routine monitoring requirements of tetrodotoxin in typical seafood.