高效液相色谱-串联质谱法测定谷物中呕吐毒素及其衍生物

目的 建立同位素稀释-高效液相色谱-串联质谱法测定谷物中呕吐毒素及其衍生物残留量的方法。 方法 样品经(86+14,v/v)乙腈水超声提取,HLB小柱净化,经C18色谱柱分离后,在质谱负离子多反应监测模式下测定。 结果 DON和3-ADON在2.0~500 μg/L,15-ADON在10.0~1 000 μg/L时,具有良好的线性关系,相关系数(r)均大于0.9990。DON及其衍生物的LOD在0.10~1.6 μg/kg之间,LOQ在0.35~6.0 μg/kg之间,加标回收率范围为80.3%~115.4%,相对标准偏差(RSD,n=6)在5.1%~14.6%之间。 结论 该方法快速简便,定量准确,可满足谷物中呕吐毒素及其衍生物的残留检测要求。

Determination of vomitoxin and its derivants in cereal grains by high performance liquid chromatography-mass spectrometry

Objective To establish the high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) with isotope dilution for the determination of vomitoxin and its derivants in cereal grains. Methods The samples were extracted with acetonitrile-H₂O(86+14,v/v),purified with HLB column, separated on a C18, and then analyzed with HPLC-MS under the negative ion multiple reaction monitoring mode. Results The linearities of DON and 3-ADON were in the concentration range of 2.0μg/L~500 μg/L, of 15-ADON in the concentration range of 10 μg/L~1000 μg/L, with the correlation coefficients higher than 0.9990. The limits of detection and the limits of quantitation were 0.10 μg/kg~1.6 μg/kg and 0.35 μg/kg~6.0 μg/kg, respectively. The average spiked recoveries ranged from 80.3% to 115.4%, and the relative standard deviation(RSD, n=6) ranged from 5.1% to 14.6%. Conclusions The high performance liquid chromatography-mass spectrometry( HPLC - MS/MS) with isotope dilution is easy, rapid and accurate. It can meet the requirements for the determination of the vomitoxin and its derivants in cereal grains.