摘要
采用液相色谱-质谱联用技术,建立了测定小麦、大麦、玉米和大米等粮食中6种脱氧雪腐镰刀菌烯醇及其衍生物的方法,并对各种粮食中的污染情况进行调查。样品采用乙腈-水（84∶16）溶液超声提取,MycosepTM 227多功能净化柱净化后,用氮气吹至近干,乙腈-0.1%氨水（5∶95）复溶,经0.22μm微孔滤膜过滤,采用负离子电喷雾电离（ESI-）,多反应监测（MRM）模式检测,外标法定量。在优化条件下,方法的线性范围为5.0～200μg/L,相关系数为0.998 8～0.999 3,检出限为0.10～0.18μg/kg。在5.0,20.0,100.0μg/kg 3个水平下的加标回收率分别为90.6%～101.6%,91.4%～99.4%和90.3%～105.0%,相对标准偏差（RSD）均小于10%。该方法具有操作简单、干扰少、快速、准确等特点,能满足国家食品风险监测方法的相关要求。
A high performance liquid chromatography-tandem mass spectrometric（ HPLC-MS /MS）method was established for the determination of six deoxynivalenols and their derivatives in grains such as wheat,barley,corn and rice. And the pollutions of those mycotoxins in grains were surveyed.The six mycotoxins in grains were extracted with acetonitrile-water（ 84 ∶ 16） in supersonic instrument,and purified with MycosepTM 227 multifuntional column. Then the purified solution was concentrated with nitrogen,and redissolved with acetonitrile-0. 1% ammonia water（ 5 ∶ 95） and cleaned with 0. 22 μm millipore filter. The filtrate was detected by HPLC-MS /MS,identified by electrospray ionization（ ESI） in negative mode using multiple reaction monitoring（ MRM） mode,and quantified by the external standard method. The calibration curves of six mycotoxins showed good linearities in the range of 5. 0-200 μg /L with correlation coefficients of 0. 998 8-0. 999 3. The detection limits of the method ranged from 0. 10 μg /kg to 0. 18 μg /kg. The recoveries of six mycotoxins at three spiked levels of 5. 0,20. 0,100. 0 μg /kg were in the ranges of 90. 6%-101. 6%,91. 4%-99. 4% and 90. 3%-105. 0%,respectively,with RSDs less than 10%. With the advantages of operation convenience,less interference from impurities and good accuracy,the method could meet the requirements of national food risk monitoring method for the determination of six deoxynivalenol in grains.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第6期660-665,共6页
Journal of Instrumental Analysis
