建立一种快速、高效测定牛奶中的呕吐毒素的免疫亲和柱-高效液相方法。样品前处理采用乙腈溶剂沉淀蛋白，用PBS缓冲液淋洗，乙腈洗脱后，洗脱液在40℃下氮吹干后，流动相复溶后检测。采用Waters RP C18色谱柱（4.6 mm×250 mm，5μm）分离，以乙腈-水（90∶10）作为流动相，用二极管阵列检测器检测，外标法峰面积定量。结果表明，呕吐毒素在0.2μg/mL~2.0μg/mL浓度范围内线性良好，相关系数r2为0.9998，检出限为0.12 mg/kg，定量限为0.40 mg/kg，加标回收率达到82.2%~98.5%。%A rapid and effective method was established for the determination of vomitoxin in milk.The samples were precipitated protein with acetonitrile, washing in PBS buffer and acetonitrile as eluent. The elution liquid was dried at 40 ℃under nitrogen, and detected after redissolved with mobile phase. The separation of target compound was performed on a Waters RP C18 chromatographic column (4.6 mm×250 mm, 5μm) using ace-tonitrile-water (90∶10) as mobile phase, with diode array detector and external standard method peak area quantification. The linear range of vomitoxin was in the range of 0.2μg/mL-2.0μg/mL with a correlation coeffi-cient of 0.999 8.The detection limit was 0.12 mg/kg and the quantitative limit was 0.40 mg/kg. The recovery rate was 82.2%-98.5%.
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