气相色谱法测定橄榄油中22种有机氯农药

GC Determination of 22 Organochlorine Pesticides in Olive Oil

橄榄油样品用乙腈提取,提取液用氮气浓缩至近干,残留物用正己烷稀释,采用硫酸磺化净化。采用气相色谱法测定样品溶液中22种有机氯农药的含量,22种有机氯农药采用Inert Cap 17色谱柱(30m×0.25mm,0.25μm)分离,电子捕获检测器测定。22种有机氯农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.001~0.01mg·kg^-1。以空白样品为基体进行加标回收试验,所得回收率为70.8%~120%,测定值的相对标准偏差(n=6)为0.40%~16%。

Olive oil sample was extracted with acetonitrile,and then the extract was evaporated to near dryness by N2-blowing.The residue was diluted with n-hexane,and purified by sulfuric acid for sulphonation.GC was applied to the determination of 22 organochlorine pesticides in the sample solution.The 22 organochlorine pesticides were separated on Inert Cap 17 chromatographic column(30 m×0.25 mm,0.25μm)and detected by ECD.Linear relationships between values of peak area and mass concentration of the 22 organochlorine pesticides were kept in definite ranges.Detection limits(3 S/N)of the method ranged from 0.001 to 0.01 mg·kg^-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 70.8%-120%,with RSDs(n=6)of determined values in the range of 0.40%-16%.