顶空/气相-质谱法测定蔬菜中1,2-二溴-3-氯丙烷含量的方法研究

Study on the Method for Determination of 1,2-dibromo-3-chloropropane Content in Vegetable by Headspace Gas Chromatography-mass Spectrometry

为了建立一种测定蔬菜中1,2-二溴-3-氯丙烷含量的检测方法。本研究采用顶空/气相色谱质谱法(HS/GC-MS/MS)进行测定,并对顶空条件进行优化和方法学验证。结果表明,适宜的顶空条件:平衡温度70℃,平衡时间30min。该方法具有良好的精密度和线性,在添加水平0.4~40μg/kg范围内,6次重复的平均添加回收率为81.83%~97.70%,RSD为4.26%~5.87%,在浓度0.1~10μg/L范围内,相关系数r^(2)为0.9994,该方法定量限为0.4μg/kg,符合分析测试质控要求。

In order to establish a method for determining 1,2-dibromo-3-chloropropane in vegetables,headspace gas chromatography-mass spectrometry(HS/GC-MS/MS)was used,which condition was optimized by setting equilibrium temperature at 70℃and equilibrium time at 30 min.The methodology was validated and showed high accuracy and good precision,with the average recoveries of 81.83%~97.70%,the relative standard deviation(RSD)of 4.26%~5.87%at fortified concentration range of 0.4~40μg/kg and the correlation coefficient of 0.9994 at concentration range of 0.1~10μg/L.The quantitation limit of 1,2-dibromo-3-chloropropane was 0.4μg/kg.Therefore,it can be concluded this method meets the requirements of quality control of analysis and test.