| 微波萃取-气相色谱/气相色谱-质谱法测定土壤中18种有机氯农药 |
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| 引用本文： | 李庆霞,刘亚轩,陈卫明,张勤.微波萃取-气相色谱/气相色谱-质谱法测定土壤中18种有机氯农药[J].岩矿测试,2010,29(2):118-122. |
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| 作者姓名： | 李庆霞 刘亚轩 陈卫明 张勤 |
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| 作者单位： | 中国地质科学院地球物理地球化学勘查研究所中心实验室,河北,廊坊,065000 |
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| 基金项目： | 中央级公益性科研院所基本科研业务费专项资金资助 |
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| 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。
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| 关 键 词： | 微波萃取 气相色谱法 气相色谱-质谱法 有机氯农药 土壤 |
| 收稿时间： | 6/4/2009 12:00:00 AM |
| 修稿时间： | 9/5/2009 12:00:00 AM |
Determination of 18 Organochlorine Pesticides in Soils by Gas Chromatography and Gas Chromatography-Mass Spectrometry with Microwave assisted Extraction |
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| LI Qing xi,LIU Ya xuan,CHEN Wei ming and ZHANG Qin.Determination of 18 Organochlorine Pesticides in Soils by Gas Chromatography and Gas Chromatography-Mass Spectrometry with Microwave assisted Extraction[J].Rock and Mineral Analysis,2010,29(2):118-122. |
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| Authors: | LI Qing xi LIU Ya xuan CHEN Wei ming and ZHANG Qin |
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| Institution: | Central Laboratory, Institute of Geophysical & Geochemical Exploration, Chinese Academy of Geological Sciences;Central Laboratory, Institute of Geophysical & Geochemical Exploration, Chinese Academy of Geological Sciences;Central Laboratory, Institute of Geophysical & Geochemical Exploration, Chinese Academy of Geological Sciences;Central Laboratory, Institute of Geophysical & Geochemical Exploration, Chinese Academy of Geological Sciences |
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| Abstract: | A sample pretreatment method of microwave-assisted extraction-Florisil solid phase extraction clean-up for gas chromatographic (GC) and gas chromatography-mass spectrometric (GC-MS) determination of the trace semi-volatile organochlorine pesticides in soils was developed. The microwave-assisted 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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| Keywords: | microwave-assisted extraction gas chromatography gas chromatography-mass spectrometry organochlorine pesticide soil |
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