基质固相分散高效液相色谱法检测河豚毒素

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。

Determination of Tetrodotoxin by MSPD-HPLC

A method was developed for extraction of tetrodotoxin from pufferfish by matrix solid phase dispersion(MSPD).The determination was carried out by high performance liquid chromatography(HPLC) with photodiode array detector(PAD) detector.Through optimizing conditions of samples pretreatment,0.5 g samples was mixed and grinded with 2.0 g strongly acidic cation exchang(SCX) sorbent with 10mL 5% ammonia∶methanol(5∶95,V/V) as eluant.The results of HPLC-PDA indicated that there was a good linear relationship for the tetrodotoxin concentration in the range of 1—100mg/L(R2=0.9990).The detection limit was 3.8ng,and quantitation detection limit was12.7ng.The recoveries were between 77.9% and 108.1% with RSD from 2.23% to 5.45%.The method is simple with short time-consuming,that can meet the requirement of detection of tetrodotoxin.