多功能柱净化-高效液相色谱法检测粮谷及其制品中的呕吐毒素  

Determination of deoxynivalenol in grain and grain products by multifunctional column clean-up and high performance liquid chromatography

作　　者：鲍蕾[1] 吴振兴[1] 石媛媛[1] 静平[1] 梁成珠[1] 

机构地区：[1]山东出入境检验检疫局技术中心,青岛266002

出　　处：《食品安全质量检测学报》2014年第3期776-782,共7页Journal of Food Safety and Quality

摘　　要：目的：建立呕吐毒素的多功能柱净化-高效液相色谱检测方法,并建立液相色谱-串联质谱确证方法。方法样品经乙腈-水溶液(84﹕16, v：v)提取、多功能柱净化、吹干、定容后,最后以液相色谱-紫外检测器进行定量分析,阳性检出以液相色谱-串联质谱法确证。结果该方法定量限为0.3μg/g,在0.5、1.0、1.5μg/g的添加水平下,样品回收率为66.0%~98.3%,室内相对标准偏差(RSDr)为1.9%~12.7%,室内HorRat值为0.1~0.7。结论该方法操作简便,灵敏度高,选择性好,适用于粮谷及其制品中呕吐毒素的检测。Objectives To establish a simple and rapid determination method of deoxynivalenol (DON) in grain and grain products by multifunctional column clean-up and high performance liquid chromatography (HPLC). Methods Samples were extracted with acetonitrile-water (84﹕16, v:v), and the extracted liquid was purified by multifunctional columns. After drying, and re-dissolved in the mobile phase, the toxins were sub-jected to HPLC-UV analysis. The positive results were confirmed using high performance liquid chromatogra-phy-tandem mass spectrometry (HPLC-MS/MS) analysis. Results Recoveries of DON added at levels ranging from 0.5 to 1.5 μg/g for all tested samples were from 66.0% to 98.3%. Relative standard deviation (RSDr) ranged from 1.9%to 12.7%. Within-laboratory HorRat values were from 0.1 to 0.7. Conclusion This method is simply clean-up, rapid and of high sensitivity, and suitable for the identification and quantification of DON in grain and grain products.

关 键 词：呕吐毒素 多功能柱 液相色谱法 液相色谱-串联质谱法 粮谷及其制品 

分 类 号：O657.63[理学—分析化学] TS210.7[理学—化学]