提出了用高分辨气相色谱-质谱法同时测定食用油中17种多氯取代以及8种多溴取代的苯并二噁英和苯并呋喃含量的方法。食用油样品依次经过酸性硅胶床、多段硅胶柱及Florisil柱净化。净化中分别用正己烷、正己烷-二氯甲烷(97+3)混合液、正己烷-二氯甲烷(40+60)和单一的二氯甲烷作为淋洗剂,洗脱上述化合物,GC-MS测定。各化合物的检出限(3S/N)在0.022 3~1.67 μg·L-1之间。用标准加入法测得多氯代化合物的回收率在97.8%~118%之间,多溴代化合物的回收率在96.5%~113%之间,测定值的相对标准偏差(n=5)分别为4.9%~6.7%和6.6%~17%之间。

HRGC-MS was applied to simultaneous determination of 17 polychloro- as well as 8 polybromo- substituted dibenzodioxins and dibenzofurans in edible oil. The oil sample was purified by passing through acid silica gel bed, multilayer silica gel column and Florisil column successively, in which eluants of n-C6H14, mixture of n-C6H14 and CH2Cl2 (97+3), mixture of n-C6H14+CH2CH2 (40+60) and CH2Cl2 in single were used respectively. The eluates used for GC-MS analysis. Detection limits (3S/N) found for the 25 compounds were in the range of 0.022 3-1.67 μg·L-1. Values of recovery found were in the ranges of 97.8%-118% with RSD′s (n=5) ranged from 4.9%-6.7% and 96.5%-113% with RSD′s (n=5) ranged from 6.6%-17%, for the polychloro-substituted compounds and polybromo-substituted compounds respectively.