建立了采用高效液相色谱-串联质谱法(HPLC-MS/MS)检测多种农产品中杀草强残留量的方法.根据样品基质不同,分别采用25%丙酮水溶液(针对小麦、鱼、肉和肝脏样品)、1%乙酸酸化的25%丙酮水溶液(针对玉米和花生样品)、1%乙酸水溶液(针对金银花、姜粉、花椒粉和茶叶样品)及1%乙酸水溶液和二氯甲烷(针对苹果、菠萝、菠菜、胡萝卜和紫苏叶)进行提取,然后依次采用二氯甲烷萃取、PCX或ENVI-Carb固相萃取柱净化后,进行HPLC-MS/MS测定,外标法定量.在0.005～0.1 mg/kg范围内,杀草强的峰面积与其质量浓度有良好的线性关系,相关系数为 0.999 7.对上述15种不同种类的农产品进行添加回收,回收率为67.5% ～98.1% ,相对标准偏差为1.0% ～9.8% .苹果、菠菜、紫苏叶、玉米、姜、鱼和肉等样品的定量限为0.01 mg/kg,茶叶、金银花、花椒粉的定量限为0.02 mg/kg.该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求.
A high performance liquid chromatography-tandem mass spectrometry method (HPLC-MS/MS) was developed for the analysis of amitrole residues in agricultural products.The samples were extracted by 25% acetone for wheat,fish,pork and liver samples,1% acetic acid-25% acetone for maize and peanut samples,1% acetic acid solution for honeysuckle,the powder of ginger,the powder of bunge prickly ash and tea leaves samples,1% acetic acid solution-dichloromethane for apple,pineapple,spinach,carrot,perilla leaves samples,respectively,followed by liquid-liquid extraction with dichloromethane.The samples were then cleaned up by PCX or Envi-Carb solid-phase extraction cartridge.The amitrole was determined and confirmed by HPLC-MS/MS.The results showed a linear relationship in the range of 0.005-0.1 mg/kg for amitrole.The correlation coefficient was 0.999 7.The average recoveries of amitrole in wheat,maize,peanut,pineapple,apple,carrot,spinach,pork,the powder of ginger,the powder of bunge prickly ash,perilla,liver,fish,honeysuckle and tea were 67.5% -98.1% .The relative standard deviations (RSDs) were 1.0% -9.8% .The limits of quantitation were 10μg/kg for wheat,maize,peanut,pineapple,apple,carrot,spinach,pork,perilla,liver,fish,honeysuckle and 20μg/kg for the powder of bunge prickly ash,the powder of ginger and tea,respectively.The method is simple,sensitive and accurate.
参考文献
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