固相萃取净化-气相色谱/串联质谱法测定茶叶中54种农药残留量  被引量:18

Determination of 54 pesticide residues in tea using solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry

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作  者:王兴宁 蔡秋 朱明 舒丹丘 刘康书 王缅 

机构地区:[1]贵州出入境检验检疫局,贵阳550004

出  处:《分析试验室》2011年第11期110-116,共7页Chinese Journal of Analysis Laboratory

摘  要:建立了固相萃取净化-气相色谱/串联质谱(SPE-GC-MS/MS)分析茶叶中54种农药残留的方法。样品用乙睛提取,提取液经石墨化炭黑/氨基固相萃取柱净化后,采用气相色谱-串联质谱方法在分时段选择反应监测模式下进行测定,外标法定量。当54种农药加标水平为10、50、100μg/kg时,回收率为60%~150%,方法的相对标准偏差小于16%;定量限(LOQ)均小于10μg/kg;在20~320μg/L范围内线性关系良好。方法已用于同时检测茶叶中农药多残留。A method was developed for simultaneous determination of 54 pesticide residues in tea using solid-phase extraction (SPE) and gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The pesticides interested were extracted from the samples with acetonitrile. The extract was purified by Carbon-PSA solid-phase extraction (SPE) cartridges. The extracts were determined by GC-MS/MS using external standard method. The recoveries for 54 pesticides in the sample spiked with the standards of 10,50,100 μg/kg were from 60 % to 150%. and the relative standard deviations were less thanl6 %. All the limits of quantification (LOQs) were less than 10 μg/kg. The linearity of the method was good between 20 and 320 μg,/L. The method is rapid,accurate,highly sensitive, and can be used for the simultaneous determination of pesticide residues in tea.

关 键 词:气相色谱-串联质谱 选择多反应监测 固相萃取 多农药残留 茶叶 

分 类 号:O657.63[理学—分析化学]

 

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