气相色谱-质谱法测定葡萄中扑灭津残留量

Determination of Propazine Residues in Grape by Gas Chromatography-Mass Spectrometry

[目的]建立了气相色谱-质谱法测定葡萄中扑灭津残留量的分析方法。[方法]样品经乙腈提取,盐析,弗罗里硅土固相萃取柱净化,气相色谱-质谱测定,选择离子监测模式,外标法定量。[结果]在0.1-4mg/kg的范围内线性良好（r〉0.99）,在0.05-0.25mg/kg的添加水平范围内,平均回收率为90%-100%,相对标准偏差（RSD）为4.7%-7.4%,检出限（LOD）为0.025mg/kg,测定低限（LOQ）为0.05mg/kg。[结论]该方法简便、快速、灵敏、准确、低成本、耐用,适合葡萄中扑灭津残留量的测定。

Objectives A gas chromatography-mass spectrometry method is presented for the quantitative determination and confirmation of propazine residues in grape.Methods Samples were extracted with acetonitrile,and an aliquot of the supernatant was cleaned up using florisil solid-phase extraction cartidges.Analyses were performed using gas chromatography-mass detection in selected ion monitoring（SIM） mode,external standards were used for quantitative determination.Results The linear range was from 0.025 to 1mg/kg.The average recoveries were 90%-100% and relative standard deviations were 4.7%-7.4% in the spiked range of 0.05-0.25mg/kg.The limit of detection were 0.005mg/kg and the limits of quantification and confirmation were 0.02mg/kg.Conclusions The method was simple,rapid,sensitive,accurate,cheap,and rugged,it was suitable for the quantitative determination and confirmation of propazine residues in grape.