建立高效液相色谱-串联质谱定量快速检测罗非鱼、南美白对虾和黄金贝中的T-2毒素与HT-2毒素方法。以10 mL乙酸乙酯作为提取溶剂,振荡提取,无水硫酸钠除水,定量移取5 mL提取液氮气吹干后用1 mL含有0.1%甲酸的甲醇-5 mmol/L乙酸铵溶液(3∶7,V/V)复溶,正己烷脱脂净化,基质匹配法外标定量。3种水产品中T-2毒素和HT-2毒素的检出限分别为2μg/kg和4μg/kg。T-2毒素质量浓度为2~100 ng/mL,HT-2毒素质量浓度为4~200 ng/mL,范围内线性良好。在3种样本中进行3个水平添加实验(n=6),T-2毒素回收率为84.3%~109.9%,HT-2毒素的回收率为90.9%~103.2%。T-2毒素的相对标准偏差为2.0%~8.7%,HT-2毒素的相对标准偏差为2.6%~10.6%。本方法简便快速、准确度好、精密度高,适用于3种代表性水产品中T-2与HT-2毒素的同时检测。
A fast high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method was developed for the quantitative determination of T-2 and HT-2 toxins in tilapia,Litopenaeus vannamei and golden scallop.After being homogenized,samples were extracted with 10 mL of neutral ethyl acetate by vibration,and after removing the moisture with sodium sulfate,5 mL of the upper layer was concentrated with nitrogen blowing,re-dissolved with 1 mL of 0.1% formic acid in methyl alcohol:5 mmol/L ammonium acetate(3:7,V/V),and degreased with hexane.The target compounds were quantified by the matrix-matched external standard method.Under optimized conditions,the lower limits of quantitation(LLOQs) for T-2 and HT-2 toxins in three aquatic products were 2 and 4 μg/kg,respectively.The linear range was 2–100 ng/mL for T-2 toxin and 4–200 ng/mL for HT-2 toxin.The average recoveries for three aquatic samples at three spiked levels ranged from 84.3% to 109.9% for T-2 toxin and 90.9% to 103.2% for HT-2 toxin.The relative standard deviations(RSDs) were in a range of 2.0%–8.7% for T-2 toxin and 2.6%–10.6% for HT-2 toxin(n = 6).The method is simple,rapid,accurate,precise and suitable for the simultaneous detection of T-2 and HT-2 toxins in the three representative aquatic products.