改良QuEChERS气相色谱法测定蔬菜中35种有机磷农药的残留量
改良QuEChERS气相色谱法测定蔬菜中35种有机磷农药的残留量
目的建立改良QuEChERS/气相色谱法测定蔬菜中35种有机磷农药残留的快速分析方法。方法样品由乙腈提取, 氯化钠盐析后, 经PSA (primary secondary amine sorbent)填料和无水硫酸镁分散固相萃取净化, 气相色谱火焰光度检测器(flame photometric detector, FDP)检测, 基质匹配标准曲线校正, 外标法定量。结果在50.0~1000.0 μg?kg-1线性范围内线性良好, 相关系数(r)为0.9959~0.9998, 在0.08、0.20、0.40 mg?kg-1 3个添加水平下35种有机磷农药的平均回收率为75.32%~118.82%, 相对标准偏差为0.46%~5.62%, 方法检出限(limit of detection, LOD)为0.01~0.05 mg?kg-1, 定量限(limit of quantitation, LOQ)为0.03~0.10 mg?kg-1。结论该方法简便快速、准确灵敏, 有机溶剂用量少, 可满足蔬菜中35种有机磷农药残留同时快速检测的实际需要。
ObjectiveTo establish a method for simultaneous analysis of 35 organophosphorous pesticide residues in vegetables by the QuEChERS-gas chromatography (QuEChERS-GC). MethodsThe samples were extracted with acetonitrile and salted out with sodium chloride. The extracts was purified by dispersive solid phase extraction using PSA and magnesium sulfate as sorbents. Gas chromatography/flame photometric detector (GC/FPD) was used for detection and matrix matching standard curve was used for correction. The external standard method was used for quantitative analysis. ResultsThirty-five kinds of organophosphorous pesticides had good linearity in the range of 50.0-1000.0 μg?kg-1 and the correlation coefficients (r) ranged from 0.9959 to 0.9998. The recoveries of 35 kinds of organophosphorus pesticides ranged from 75.32% to 118.82%, with relative standard deviations (RSDs) from 0.46% to 5.62% at 3 spiked levels of 0.08、0.20、0.40 mg?kg-1. The limits of detection (LOD) were in range of 0.01-0.05 mg?kg-1. The limit of quantitation (LOQ) were in range of 0.03-0.10 mg?kg-1. ConclusionThis method is simple, rapid, sensitive, with a small amount of organic solvent, which can meet the demands for the simultaneous determination of multi-residue organophosphorous pesticide residues in vegetables.
标题：改良QuEChERS气相色谱法测定蔬菜中35种有机磷农药的残留量
英文标题：Determination of 35 kinds of organophosphorous pesticide residues in vegetables by modified QuEChERS/gas chromatography
作者：
杨坤 贵州省黔东南州食品药品检验检测中心
龙姜柳 贵州省黔东南州食品药品检验检测中心
周曦曦 贵州省黔东南州民族医药研究院
李丽 凯里学院环境与生命科学学院
张建炀 贵州省黔东南州食品药品检验检测中心
中文关键词:QuEChERS,气相色谱法,蔬菜,有机磷农药,
英文关键词:QuEChERS,gas chromatography,vegetables,organophosphorous pesticide,
发表日期：2018-12-13
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