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固相萃取净化-气相色谱-质谱法测定鳗鱼中多种农药残留量

Determination of multi Pesticide Residues in Eels by GC-MS coupled with Solid Phase Extraction
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摘要 建立了固相萃取-气相色谱串联质谱法检测鳗鱼中丁烯氟虫腈、三氯杀蟎醇等20种农药残留的分析方法。试样经乙腈提取后加入适量的去离子水和正己烷除去水溶性杂质和脂溶性杂质,再经填有中性氧化铝、C18和PSA混合填料的自组装固相萃取柱净化后进行GC-MS检测分析。采用选择离子扫描方式,用内标法进行定量。本方法简便、快速,方法的检出限(S/N=3)为0.001~0.009 mg/kg,在加标水平为0.01 mg/kg时,平均回收率为70.7~120%,相对标准偏差(RSD)为2.9~7.2%;在加标水平为0.02 mg/kg时,平均回收率为70.3~120%,相对标准偏差(RSD)为2.9~6.2%。 A method for the determination of multi pesticide multiresiduals such as flufiprole, dicofol in eels by gas chromatography with solid-phase extraction was proposed. The compounds were extracted from homogenized tissue with acetonitrile. Water-soluble and fat-soluble impurities in acetonitrile was removed by a moderate amount of hexane and deionized water. Acetonitrile extract purified by self-assembly solid-phase extraction column with mixed power of Alumina-N, C18 and PSA was ready for GC-MS analysis. The determination was performed in selected ion monitoring(SIM) mode with inner standard method for quantitative analysis. The detection limits(S/N=3)were in the range of 0.001-0.009 mg/kg.Tests for recovery were made by addition of mixed standards of 0.01 mg/kg,and the results were 70.7-120%,and the relative standard deviations were 2.9-7.2%. Tests for recovery were made by addition of mixed standards of 0.02 mg/kg,and the results were 70.3-120%,and the relative standard deviations were 2.9-6.2%.
出处 《福建分析测试》 CAS 2013年第6期28-31,36,共5页 Fujian Analysis & Testing
基金 福建检验检疫局科技计划项目:FK2011-52
关键词 固相萃取 气相色谱-质谱 农药残留 鳗鱼 三氯杀蟎醇 Solid-Phase Extraction(SPE) GC-MS Pesticide Residues Eels Dicofol.
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