凝胶渗透色谱－液相色谱－串联质谱法测定水产品中性激素

建立水产品中性激素的凝胶渗透色谱净化－超高效液相色谱－串联质谱分析方法。采用乙酸乙酯提取样品，经GPC净化后， LC－MS／MS测定，外标法定量。流动相为乙腈和0．1％甲酸水溶液，梯度洗脱，电喷雾正离子多反应模式监测。3种性激素在0．5～20．0μg／L线性范围内，相关系数大于0．998，定量限为0．3μg／kg，回收率为88．6％～96．4％，相对标准偏差为1．84％～6．24％。本方法灵敏度高、重现性好，适用于水产品中性激素的测定。

Determination of Hormones in Aquatic Products by HPLC-MS with Gel Permeation Chromatography

A method was developed for hormones in aquatic products by high performance liquid chromatography-mass spectrometry （ HPLC-MS） with gel permeation chromatography.The samples were extracted by ethyl acetate and cleaned up with GPC. The analysis was carried out on LC-MS/MS and external standard method was used for quantification.The chromatographic separation was performed with gradient elution by using acetonitrile and 0.1%formic acid solution as mobile phase.Detection was carried out by electrospray positive ionization mass spectrometry in the multiple reaction monitoring mode.Linear ranges of three hormones were in the range of 0.5~20.0μg/L with correlation coefficient more than 0.998.The quantification limits of the method were 0.3 μg/kg.The recovery of tetrodotoxin was 88.6%~96.4%, and the relative standard deviations were 1.84%~6.24%.The method could be used to identify and quantify hormones in aquatic products with satisfactory sensitive and reproducible.