| 加速溶剂萃取-气相色谱/质谱法同时测定土壤中拟除虫菊酯类等18种农药残留 |
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| 引用本文： | 李俊,肖雅雯,王震,赵为武.加速溶剂萃取-气相色谱/质谱法同时测定土壤中拟除虫菊酯类等18种农药残留[J].岩矿测试,2011,30(5):590-595. |
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| 作者姓名： | 李俊 肖雅雯 王震 赵为武 |
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| 作者单位： | 贵州省农产品质量安全监督检验测试中心;华南农业大学资源环境学院; |
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| 摘 要： | 采用正己烷-丙酮-磷酸混合溶剂为提取剂,在萃取温度100℃、压力10.3 MPa条件下,用快速溶剂萃取仪提取土壤样品,石墨碳黑氨基固相萃取柱净化,PTV大体积进样,气相色谱-质谱联法同时检测六六六(HCHs)、滴滴涕(DDTs)和10种拟除虫菊酯类农药(联苯菊酯、甲氰菊酯、氯氟氰菊酯、氯菊酯、氯氰菊酯、氟氯氰菊酯、氟氨氰菊酯、氰戊菊酯、氟氰戊菊酯、溴氰菊酯)共18种农药残留。在10～20μg/kg的添加浓度下,目标化合物平均回收率为82.84%～96.33%,相对标准偏差(RSD,n=6)为3.21%～7.34%;在20～40μg/kg的添加浓度下,目标化合物平均回收率为80.55%～103.76%,RSD(n=6)为2.56%～5.78%;在40～80μg/kg的添加浓度下,目标化合物平均回收率81.56%～95.38%,RSD(n=6)为2.19%～5.88%。方法检出限为0.11～3.40μg/kg,实际样品检测的RSD(n=3)为4.94%～8.74%。方法简单快速、灵敏度高、准确度好,可以满足土壤中HCHs、DDTs和拟除虫菊酯类农药残留的实际检测需要。
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| 关 键 词： | 土壤 拟除虫菊酯类 六六六 滴滴涕 快速溶剂萃取 气相色谱-质谱法 |
| 收稿时间： | 2010/12/14 0:00:00 |
| 修稿时间： | 2011/3/17 0:00:00 |
Simultaneous Determination of 18 Pesticide Residues including Pyrethroids in Soils by Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction |
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| LI Jun,XIAO Ya-wen,WANG Zhen and ZHAO Wei-wu.Simultaneous Determination of 18 Pesticide Residues including Pyrethroids in Soils by Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction[J].Rock and Mineral Analysis,2011,30(5):590-595. |
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| Authors: | LI Jun XIAO Ya-wen WANG Zhen and ZHAO Wei-wu |
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| Institution: | LI Jun1,XIAO Ya-wen2,WANG Zhen1,ZHAO Wei-wu1*(1.Supervision and Testing Center for Agri-Produce Quality and Safety of Guizhou Province,Guiyang 550004,China,2.College of Natural Resources and Environment,South China Agricultural University,Guangzhou 510642,China) |
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| Abstract: | A method was developed for simultaneous determination of 18 pesticide residues in soils,including hexachlorocyclohexanes(HCHs),dichlorodiphenyltrichloroethanes(DDTs) and other 10 kinds of pyrethroid.The soil samples were distilled with Accelerated Solvent Extraction(ASE) and extracted by hexane-acetone-H3PO4 at extraction temperature of 100℃ and pressure of 10.3 MPa.The distilled solutions were purified by solid phase extraction(SPE).The purified solutions were injected into Gas Chromatography-Mass Spectrometry(GC-MS) by using programmed temperature vaporization(PTV) and large volume injector(LVI).If the spiked level was 10-20 μg/kg,the recoveries of target compounds were 80.55%-96.33% and the relative standard deviations(RSDs,n=6) were 3.21%-7.34%.If the spiked level was 20-40 μg/kg,the recoveries were 80.55%-103.76% and RSDs(n=6) were 2.56%-5.78%.If the spiked level was 40-80 μg/kg,the recoveries were 81.56%-95.38%,RSDs(n=6) were 2.19%-5.88%.The method detection limits were 0.11-2.38 μg/kg,RSDs(n=3) were 4.94%-8.74% for real samples.The method is simple and rapid with high sensitivity making it suitable for simultaneous determination of residues of benzex and DDTs and pyrethroid in soils. |
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| Keywords: | soil pyrethroids hexachlorocyclohexanes(HCHs) dichlorodiphenyltrichloroethanes(DDTs) accelerated solvent extraction gas chromatography-mass spectrometry |
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