高效液相色谱-紫外法同时检测小麦中DON、15ACDON和3ACDON

建立了测定小麦中B型单端孢酶烯族毒素脱氧雪腐镰刀菌烯醇(deoxynivalenol, DON)、3-乙酰脱氧雪腐镰刀菌烯醇(3-acetyldeoxynivalenol, 3-ACDON)和15-乙酰脱氧雪腐镰刀菌烯醇(15-acetyldeoxyni-valenol, 15-ACDON)的高效液相色谱-紫外(HPLC-UV)检测方法。用水提取小麦样品，提取液经无水乙醇等体积沉淀，再结合Oasis HLB固相萃取小柱可取得较好的净化效果。采用乙腈/0.005%磷酸水溶液二元梯度洗脱程序在高效液相色谱-紫外检测器上完成DON、15ACDON和3ACDON的定性定量分析。结果表明，在0.5~15.0 mg L^-1线性范围内，DON、15ACDON和3ACDON的平均加标回收率分别为89.8%、93.4%和92.9%，相对标准偏差分别为2.2%、2.0%和2.5% (n=3)；检测限分别为12.2、10.5和16.7 μg kg^-1。该方法准确、重现性好，样品净化方法使杂峰干扰少，大幅减少有机溶剂的使用，成本低，适用于小麦中B型单端孢酶烯族毒素的大批量检测。

Establishment of a HPLC-UV Method for Simultaneous Determination of DON, 15ACDON, and 3ACDON in Wheat

A HPLC-UV method was established to determine deoxynivalenol (DON), 3-acetyldeoxynivalenol (3-ACDON) and 15- acetyldeoxynivalenol (15-ACDON) in wheat. Wheat sample was extracted by water, and the extracting solution was precipitated with an equal volume of ethanol followed by solid phase extraction with Oasis HLB cartridge. Qualitative and quantitative analyses of DON, 15ACDON and 3ACDON were done by HPLC-UVD using gradient elution program with acetonitrile and 0.005% phosphoric acid solution. Results showed that at the linear range of 0.5–15.0 mg L^-1, the recoveries were 89.8%, 93.4%, and 92.9%, respectively. The relative standard deviations were 2.2%, 2.0%, and 2.5%, respectively, and the detection limit levels were 12.2, 10.5, and 16.7 μg kg^-1, respectively. The method was accurate and reproducible. Sample purification lessened interference peaks, and due to the use of organic solvents was greatly reduced, the cost was decreased. Therefore, the method was suitable for the large batch determination of type B trichothecenes in wheat.