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建立了河豚鱼肉中河豚毒素的基质固相分散萃取的提取方法,并采用高效液相色谱-二极管阵列检测器进行测定。通过样品前处理的优化,确立选取0.5g样品与2.0g阳离子交换(SCX)吸附剂混合研磨,并采用10mL 5%氨水:甲醇溶液(5:95,V/V)作为洗脱剂。经HPLC-PDA检测,结果表明,河豚毒素在1—100mg/L浓度范围内呈现良好的线性关系(R2=0.9990),检出限为3.8ng,定量下限为12.7ng;加标回收率为77.9%—108.1%,RSD为2.23%—5.45%。该方法操作简单、耗时少,符合河豚毒素分析检测的要求。
A method for the determination of tetrodotoxin in Puffer fish by matrix solid-phase dispersion extraction was established and determined by high performance liquid chromatography-diode array detector. Through optimization of sample pretreatment, 0.5g sample was selected and mixed with 2.0g cation exchange (SCX) adsorbent and ground with 10mL of 5% aqueous ammonia: methanol solution (5: 95, V / V) as eluent. The results of HPLC-PDA showed that the concentration of tetrodotoxin showed a good linear relationship (R2 = 0.9990) in the range of 1-100mg / L with the detection limit of 3.8ng and the lower limit of quantitation of 12.7ng. The spiked recoveries were 77.9 % -108.1%, RSD 2.23% -5.45%. The method is simple, less time-consuming, in line with tetrodotoxin analysis and detection requirements.