基于N-丙基乙二胺键合硅胶和十八烷基键合锆胶的QuEChERS-气相色谱-质谱法检测酥油中的8种有机磷农药残留

Determination of 8 kinds of organophosphorus pesticide residues in butter by QuEChERS-gas chromatography-mass spectrometry based on primary secondary amine and C18-bonded zirconium rubber

中文关键词:  酥油  净化剂  气相色谱-质谱法  有机磷农药

英文关键词:butter  cleaning agent  gas chromatography-mass spectrometry  organophosphorus pesticide

中文摘要:

      目的 建立一种基于N-丙基乙二胺键合硅胶(primary secondary amine, PSA)和十八烷基键合锆胶(C18-bonded zirconium rubber, Z-sep+)为净化材料的QuEChERS-气相色谱-质谱法检测酥油中的8种有机磷农药残留的分析方法。方法 使用乙腈对样品中的农药残留进行提取, 以PSA和Z-sep+为QuEChERS净化材料, 对提取液中的干扰物质进行去除, 净化后的样品进气相色谱-质谱联用仪检测。结果 在线性范围10~500 μg/kg内, 目标定量离子峰面积与相应浓度呈良好的线性关系, 相关系数r>0.99, 检出限(limit of detection, LODs)为1.08~7.16 μg/kg, 定量限(limit of quantitation, LOQs)为3.59~23.86 μg/kg, 以25、100和500 μg/kg浓度水平添加回收率为73.6~113.1%, 相对标准偏差(relative standard deviation, RSD)位于5.1~17.2%, 日内精密度和日间精密度满足实验要求。结论 该方法快速、准确、灵敏, 适合测定酥油中有机磷农药残留。

英文摘要:

      Objective To establish a method for the determination of 8 organophosphorus pesticide residues in butter by QuEChERS-gas chromatography-mass spectrometry based on PSA (primary secondary amine) and Z-sep+(C18-bonded zirconium rubber) as clean-up materials. Methods After the pesticide residues were extracted by acetonitrile, PSA and Z-sep+ were used as QuEChERS clean-up agents to remove the interfering substances in the extract, and the purified samples were detected by GC-MS. Results In the linear range of 10~500 μg/kg, the peak area of the target quantitative ion had good linear relationship with the corresponding concentration r>0.99, LODs (limit of detection) were 1.08?7.16 μg/kg, LOQs (limit of quantitation) were 3.59?23.8 μg/kg, the recoveries were 73.6?11.31% at the concentration of 25, 100 and 500 μg/kg, and the RSDs were 5.1?17.2%. The intra-day precision and inter-day precision met the experimental requirements. Conclusion This method is rapid, accurate, sensitive and suitable for the determination of organophosphorus pesticide residues in butter.