超高效液相色谱-串联质谱法同时测定玉米和小麦中玉米赤霉烯酮和玉米赤霉烯酮-14-葡萄糖苷检测方法的建立

Development of a UHPLC-MS/MS method for simultaneous determination of zearalenone and zearalenone-14-glucoside in maize and wheat

为科学防控和保障粮食质量安全,以玉米和小麦为材料,用乙腈/水/甲酸溶液提取,经HLB固相萃取柱净化,采用基质匹配标准溶液进行准确定量,建立了一种可靠的超高效液相色谱-串联质谱(UHPLC-MS/MS)方法,用于同时测定玉米和小麦中玉米赤霉烯酮(ZEN)和玉米赤霉烯酮-14-葡萄糖苷(ZEN-14G)。结果表明:ZEN和ZEN-14G在0.1—200μg/L范围内呈良好线性关系(R^(2)>0.999),检出限为0.03—0.3μg/kg,定量限为0.1—1.0μg/kg。在20、50μg/kg和100μg/kg三种添加水平下,回收率为(80.2±9.8)%—(98.6±4.2)%,精密度为0.2%—9.1%(n=5)。该方法准确、灵敏度高,可以满足玉米和小麦中ZEN和ZEN-14G的检测要求。

To scientifically control and ensure food quality and safety,maize and wheat were used as materials,extracted with acetonitrile/water/formic acid solution,purified by HLB solid-phase extraction column,and accurately quantified by matrix matching standard solution,and a reliable ultra-high performance liquid chromatography-mass spectrometry(UHPLC-MS/MS)method was established for simultaneous determination of zearalenone(ZEN)and zearalenone-14-glucoside(ZEN-14G)in maize and wheat.The results showed that ZEN and ZEN-14G exhibited a good linear relationship in the range of 0.1200μg/L(R^(2)>0.999),with a detection limit of 0.03—0.3μg/kg and a quantification limit of 0.1—1.0μg/kg.At three levels of addition of 20,50μg/kg,and 100μg/kg,the recovery rate was(80.2±9.8)%—(98.6±4.2)%,and the precision was 0.2%-9.1%(n=5).This method is accurate,highly sensitive,and can meet the detection requirements of ZEN and ZEN-14G in maize and wheat.