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

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

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．O-500μg／L，15-ADON在10．0～1000μg/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—1．6μg/kg之间，LOQ在0．35—6．0μg／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。

Objective To establish the high performance liquid chromatography-mass spectrometry （HPLC-MS/MS） with iso- tope dilution for the determination of vomitoxin and its derivants in cereal grains. Methods The samples were extracted with acetonitrile-H2 O（ 86＋ 14, v/v ） , purified with HLB column, separated on a C 18, 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- 1.6μg/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.