多功能柱净化-高效液相色谱法同时检测小麦中雪腐镰刀菌烯醇和脱氧雪腐镰刀菌烯醇  被引量:10

Simultaneous Determination of Nivalenol and Deoxynivalenol in Wheat by High Performance Liquid Chromatography Using Multifunctional Clean-up Column

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作  者:隋凯[1] 李军[1] 卫锋[1] 

机构地区:[1]辽宁出入境检验检疫局,辽宁大连116001

出  处:《分析测试学报》2006年第3期56-59,共4页Journal of Instrumental Analysis

摘  要:建立了小麦中雪腐镰刀菌烯醇(NIV)和脱氧雪腐镰刀菌烯醇(DON)的高效液相色谱同时检测方法。样品采用乙腈-水(体积比85:15)混合溶剂进行提取.通过多功能净化柱(MFC)进行一次性净化,以C18柱为分离柱,水-乙腈-甲醇(体积比90:5:5)混合溶剂为流动相进行高效液相色谱分离和检测。在小麦样品中,本方法在0.2~5μg/g添加范围内的凹收率为87%~99%;相对标准偏差为1.5%~8.3%;DON和NIV的检出限分别为0.12和0、16μg/g(5/N=3)。A HPLC method for simultaneous determination of deoxynivalenol (DON) and nivalenol (NIV) in wheat was developed. After extracting the sample with a mixture of acetonitrile - water(85 : 15 by volume), the extract was one-time purified by multifunctional clean-up column. DON and NIV were then separated and determined by reversed-phase HPLC with Symmetry^R C18 column and a mixture of water-acetonitrile- methanol(90 : 5 : 5 by volume) as mobile phase. The linear range for DON was 0. 5 - 10 mg/L with a correlation coefficient of 0. 998 8 and that for NIV was 0. 5 - 10 mg/L with a correlation coefficient of 0. 999 1. The deteetion limits for DON and NIV were 0. 12 and 0. 16μg/g (S/N= 3) , respectively. The recovery ranges tbr DON and NIV were 92% - 96% and 87% - 99% , respectively, and their standard deviation range was 1.5% -8.3%.

关 键 词:雪腐镰刀菌烯醇(NIV) 脱氧雪腐镰刀菌烯醇(DON) 多功能净化柱(MFC) 高效液相色谱 

分 类 号:O657.72[理学—分析化学] S432.41[理学—化学]

 

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