多功能净化柱-高效液相色谱法检测玉米油中呕吐毒素

Determination of deoxynivalenol in corn oil by HPLC with multifunctional purification column

研究建立了多功能净化柱-高效液相色谱法检测玉米油中呕吐毒素(DON)的方法。样品经乙腈-水(体积比80∶20)混合溶剂振荡提取、超声波辅助萃取、多功能净化柱净化处理后,以乙腈-水(体积比16∶84)为流动相进行高效液相色谱检测。结果表明:DON在质量浓度为0.01~5μg/m L范围内具有良好的线性关系;线性方程为y=63 626.6x+390.1,相关系数为0.999 97,检出限(S/N)为3μg/kg;3个不同水平平均加标回收率为87.6%~104.8%,相对标准偏差为1.8%~5.3%。该方法可在8 min内完成检测、重现性好、灵敏度高,对取自不同工厂的13个成品玉米油样品进行检测,DON含量均低于国标限量(1 000μg/kg)。

A method for determination of deoxynivalenol （DON） in corn oil was established lay HPLC witn muhifunctional purification column. The sample was oscillatorily extracted by acetonitrile -water（ volume ratio 80： 20）, extracted with ultrasound assist and purified by multifunctional purification column, then determined by HPLC with acetonitrile- water（ volume ratio 16： 84）as mobile phase. The results showed that there was a good linear relationship when the mass concentration of DON was 0.01 -5 i^g/mL,and the linear equation was y = 63 626.6x ＋ 390.1, the correlation coefficient was 0.999 97, and the limit of detection （S/N）was 3 μg/kg. The mean recoveries and relative standard deviations in three levels were 87.6% - 104.8% and 1.8% - 5.3%, respectively. The method could complete determination within 8 min with good repeatability and high sensitivity. Thirteen corn oils samples from different factories were detected by the method, and the results showed that the contents of DON in all the samples were lower than the national standard limitation （1 000 μg/kg）.