CAJ | 학술논문

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。
목적：건립구토독소적다공능주정화-고효액상색보검측방법,병건립액상색보-천련질보학증방법。방법양품경을정-수용액(84﹕16, v：v)제취、다공능주정화、취간、정용후,최후이액상색보-자외검측기진행정량분석,양성검출이액상색보-천련질보법학증。결과해방법정량한위0.3μg/g,재0.5、1.0、1.5μg/g적첨가수평하,양품회수솔위66.0%~98.3%,실내상대표준편차(RSDr)위1.9%~12.7%,실내HorRat치위0.1~0.7。결론해방법조작간편,령민도고,선택성호,괄용우량곡급기제품중구토독소적검측。
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.