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

中文关键词:  呕吐毒素  多功能柱  液相色谱  粮谷及其制品  液相色谱-串联质谱

英文关键词:DON  multifunctional column  High Performance Liquid Chromatography  Grain and Grain Products  HPLC/MS/MS

中文摘要:

      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0.3 μg/g, 在0.5、1.0、1.5 μg/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。

英文摘要:

      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 subjected 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 rang-ing 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.