DON净化柱——高效液相色谱法检测粮谷中呕吐毒素

DETERMINATION OF DEOXYNIVALENOL IN GRAINS BY HPLC USING DON CLEAN-UP COLUMN

通过自制DON净化柱和高效液相色谱仪,建立了检测谷物中呕吐毒素的方法。样品经乙腈—水溶剂提取后,通过自制的DON净化柱净化,采用C18分离柱和紫外检测器测定。结果表明:样品通过乙腈—水(体积比V/V,84∶16)混合溶剂和超声20min的提取,可大幅度提高方法回收率;呕吐毒素在0.5mg/kg～8.0mg/kg内线性关系好,相关系数为0.999;在0.5、2.0和8.0mg/kg的加标水平下,回收率为95.1%～102.3%,相对标准偏差为1.8%～6.4%,检出限(信噪比)为50μg/kg。

A method was developed for the determination of deoxynivalenol in Grains by high performance liquid chromatographic（HPLC） method.The samples of Grains were extracted with aceronitrile-water mixture（84/16,V/V）and cleaned up by homemade DON Clean-up Columns.Then,the extracts were separated with C18 column and analyzed by UV detector.The result showed that the recovery rate was greatly increased,when the extraction by using supersonic waves for 20 minters.Linear range of DON was 0.5～8.0 mg/kg with correlation coefficient of 0.999.The average recovery at the spiked levels of 0.5,2.0 and 10.0 mg/kg for grains were from 95.1% to 102.3%,and relative standard deviations were from 1.8% to 6.4%.The detection limit（S/N= 3） was 50μg/kg for deoxynivalenol.