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建立了同位素稀释-高分辨气相色谱/高分辨质谱法(HRGC/HRMS)测定南极土壤、苔藓和地衣样品中23种有机氯农药的分析方法.样品经冷冻干燥、研磨处理后用正己烷∶二氯甲烷(1∶1,V∶V)混合溶剂进行加速溶剂萃取(ASE),萃取液经硅胶-氧化铝层析柱和C18小柱净化后,进HRGC/HRMS检测分析.样品中目标物定量采用平均相对响应因子法,6点标准曲线响应因子的相对标准偏差(RSD)≤20%,方法的线性范围为0.4—800μg·L-1,回收率在62%—101%之间.实际样品分析结果表明,23种OCPs的加标回收率为40%—100%,在土壤、苔藓和地衣样品中的检出限(LODs)分别为0.024—5.01、0.2—12.2、0.020—13.7 pg·g-1,可以满足南极环境样品中有机氯农药的检测分析.
An analytical method was established for determination of 23 organochlorine pesticides in Antarctic soil, moss and lichen samples by isotope dilution-high resolution gas chromatography / high resolution mass spectrometry (HRGC / HRMS). The samples were freeze-dried and ground with n-hexane: Accelerated solvent extraction (ASE) was carried out with mixed solvent of methyl chloride (1: 1, V: V) and the extract was purified by silica gel-alumina column and C18 column and analyzed by HRGC / HRMS. The relative standard deviation (RSD) of 6-point standard curve response factor (RSD) was less than or equal to 20% using the average relative response factor method, the linear range was 0.4-800μg · L-1 and the recovery was between 62% and 101% The results showed that the recovery of 23 OCPs was 40% -100%, and the detection limits (LODs) in soil, moss and lichen were 0.024-5.01,0.2-12.2,0.020-13.7 pg · g -1, which can meet the detection and analysis of organochlorine pesticides in Antarctic environmental samples.