摘要:
采用微波萃取-Florisil固相萃取柱净化分离、气相色谱和气相色谱-质谱相结合的方法测定土壤中的痕量半挥发性有机氯农药。优化了微波萃取和固相萃取柱净化条件，在最优条件下18种有机氯农药（α-HCH、β-HCH、γ-HCH、δ-HCH、七氯、艾氏剂、环氧七氯、硫丹Ⅰ、p,p′-DDE、狄氏剂、异狄氏剂、硫丹Ⅱ、p,p′-DDD、o,p′-DDT、异狄氏剂醛、硫丹硫酸酯、p,p′-DDT、甲氧滴滴涕）的回收率在89.56%～114.22%。对气相色谱和气相色谱-质谱法的仪器检出限、回收率、精密度和方法检出限进行对比，确定了采用气相色谱-质谱定性和气相色谱定量相结合的方法，测定实际土壤样品中的有机氯农药，使得定性和定量的准确度都得到提高。
Abstract:
A sample pretreatment method of microwaveassisted extractionFlorisil solid phase extraction cleanup for gas chromatographic (GC) and gas chromatographymass spectrometric (GC-MS) determination of the trace semivolatile organochlorine pesticides in soils was developed. The microwaveassisted extraction and Florisil solid phase extraction conditions were optimized. Under the optimum condition, the recoveries of 18 organochlorine pesticides (α-HCH, β-HCH, γ-HCH, δ-HCH, heptachlor, aldrin, heptachlor epoxide, endosulfan Ⅰ, p,p′-DDE, dieldrin, endrin, endosulfan Ⅱ, p,p′-DDD, o,p′-DDT, endrin aldehyde, endosulfan sulfate, p,p′-DDT, methoxychlor) were 89.56%～114.22%. The instrument detection limit, recovery, precision and detection limit of method were compared between GC and GC-MS. Based on the combination of sample pretreatment method with GC (for quantitative determination) and GC-MS (for qualitative determination) determination, an analytical system for the determination of 18 organochlorine pesticides in soils was established and has been applied to the determination of organochlorine pesticides in soil samples with satisfactory results.
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