气相色谱-三重四极杆串联质谱法测定富勒烯中痕量苯残留

Determination of trace benzene residue in C_(60) and C_(70) fullerenes by GC-MS/MS

采用气相色谱-三重四极杆串联质谱法(GC-MS/MS),建立了适用于C_(60)、C_(70)富勒烯中的痕量苯残留的分析测试方法。研究结果表明,在3~400μg/L浓度范围内本方法具有良好线性关系,线性相关系数为0.9999;检出限与定量限值分别为9μg/kg和30μg/kg,系统适应性的RSD%值为0.95%,具有良好的专属性和重复性。C_(60)、C_(70)富勒烯重复性检测结果的RSD%值分别为4.81%和1.35%;中间精密度良好,不同时间且不同人员在同一台仪器上测定C_(60)、C_(70)富勒烯结果的RSD%值分别为4.48%和1.25%。本方法的加标回收率为94.39%~96.45%,对应的RSD%值为1.15%~1.41%。采用3种市售C_(60)富勒烯和2种C_(70)富勒烯样品进一步对本方法进行了验证,均未检测出苯残留。本方法选择性好、灵敏度高、分析速度快,操作便捷且检测成本低,可广泛应用于C_(60)、C_(70)富勒烯中痕量苯残留的检测。

The test results showed that the standard curve was obtained with good linear correlation coefficient(r 2=0.9999)in the concentration range of 3-400μg/L.The limits of detection and quantitation were 9μg/kg and 30μg/kg,respectively.The RSD%value of system suitability was 0.95%,showing good specificity and repeatability.The RSD%values of detection results of repeatability for C_(60) and C_(70) fullerenes were 4.81%and 1.35%,respectively.The intermediate precision was good,at different time,the RSD%values of C_(60) and C_(70) fullerene results measured on the same instrument by different test personnel were 4.48%and 1.25%,respectively.The recovery rates of the method were 94.39%-96.45%,and the corresponding RSD%values ranged from 1.15%to 1.41%.Benzene residue was not detected in three kinds of C_(60) fullerenes and two kinds of C_(70) fullerenes.This method has advantages of good selectivity,high sensitivity,fast analysis speed,convenient operation,low detection cost,high accuracy and good reliability.