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固相萃取法萃取葡萄酒中赭曲霉毒素A的方法研究
谢春梅1, 李倩倩2, 王 华1
1.西北农林科技大学 葡萄酒学院;2.西北农林科技大学 食品科学与工程学院
摘要:
【目的】建立葡萄酒中赭曲霉毒素A(Ochratoxin A,OTA)的固相萃取方法。【方法】分析了固相萃取小柱的活化方法、淋洗液、洗脱溶剂对萃取葡萄酒中OTA的影响,选择出最佳的参数后进行精密度与准确度试验。【结果】葡萄酒中OTA的固相萃取方法:C18固相萃取柱(简称C18-SPE柱)经5 mL甲醇、5 mL双蒸水活化后,进样10 mL,先用1 mL双蒸水淋洗,充分干燥后,用5 mL乙酸乙酯洗脱,收集洗脱液并真空旋转蒸发至干,1 mL流动相溶解残渣待测。【结论】得到了萃取葡萄酒中OTA的固相萃取方法,此方法的平均回收率为88.2%~100.9%,变异系数为0.93%~2.19%,且具有操作简单,成本低,分析速度快等优点。
关键词:  赭曲霉毒素A  葡萄酒  固相萃取  乙酸乙酯
DOI:
分类号:
基金项目:陕西省“13115”科技创新工程重大科技专项计划项目(2007ZDKG-09)
Research on solid-phase extraction of ochratoxin A from wine
Abstract:
【Objective】 A basic method of Solid-phase Extraction(SPE) for extracting Ochratoxin A (OTA) from wine was established.【Method】 Factors,including various ways of activity,washing solution,elution,on extracting Ochratoxin A were valued and simultaneously suitable related parameters were selected and evaluated for precision and accuracy.【Result】 10 mL wine was firstly brought into the C18 cartridge which was previously activated by 5 mL methanol and 5 mL water,later,flushed with 1mL water,then,after entirely dried,eluted with 5 mL ethyl acetate. The eluent was collected and evaporated till dry,and the residue was dissovled with 1 mL of mobile phase for determination.【Conclusion】 The recoveries of this method were between 88.2% and 100.9%, and coefficient of variation varied from 0.93% to 2.19%.This method is characterized with an ideal attribute of simplicity,low cost and rapid analysis.
Key words:  Ochratoxin A  wine  solid-phase extraction  ethyl acetate