改进的分散固相萃取-气相色谱-质谱联用法测定蘑菇罐头中57种农药残留
Determination of 57 pesticide residues in canned mushrooms by modified dispersive-solid phase extraction-gas chromatography-mass spectrometry
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摘要: 建立了改进的分散固相萃取(d-SPE)-气相色谱-质谱联用法测定蘑菇罐头中57种农药残留的方法。首次将石墨烯作为分散固相萃取的净化剂应用到蘑菇罐头的农药残留检测中,与传统的PSA+C18吸附剂组合相比,石墨烯具有除杂效果好和成本低的优点。本文采用外标法定量,57种农药在0.010.5mg/L范围内线性良好,线性系数在0.9870.9998之间,除氟虫腈外,大多数农药的3个水平的加标回收率在70.2%130%之间,精密度(n=5)小于10%,检出限(LOD)为0.819.7μg/kg。结果表明,该方法适合于蘑菇罐头中农药残留的检测。Abstract: A quick method was established for the determination of 57 pesticide residues in canned mushrooms by by gas chromatography with mass spectrometry(GC-MS) after modified dispersive solid-phase extraction(d-SPE). Graphene as d-SPE sorbent firstly was applied on the determination of 57 pesticide residues in canned mushrooms. Compared with previous primary-secondary amine(PSA) and octadecylsilance(ODS),graphene had advantage of effective impurity removal and low cost. The experiment was quantitative using external standard method and showed a good linearity over the ranger of 0.987~0.9998. The recoveries of most pesticides were from 70.2% to 130% except Fipronil and precision(n=5) were less than 10%,and the detection limit of 57 pesticides were from 0.8~19.7μg/kg. The result indicated that the developed method was suitable for the determination of 57 pesticide residues in canned mushrooms.