基于QuEChERS-气相色谱-串联质谱法测定鸡蛋中48种农药残留

Determination of 48 pesticide residues in eggs by QuEChERS-gas chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  气相色谱-串联质谱  鸡蛋  农药残留

英文关键词:QuEChERS  gas chromatography-tandem mass spectrometry  eggs  pesticide residues

中文摘要:

      目的 建立基于QuEChERS前处理方法结合气相色谱-串联质谱测定鸡蛋中48种农药残留的检测方法。方法 样品用1%乙酸乙腈、MgSO4和NaOAC混合盐包脱水提取, 经MgSO4、PSA、GCB和C18混合净化管净化, 净化液经氮吹浓缩后乙酸乙酯定容, 利用气相色谱分离, MRM模式测定, 内标校正, 外标法定量。 结果 48种农药在线性范围为5~100 ng/mL内关系良好, r2均在0.995以上。方法检出限在0.03~5.00 μg/kg之间, 方法定量限在0.12~17.00 μg/kg之间。48种农药在5、10和50 μg/kg 3个加标水平上, 平均回收率在70%~120%的占比分别为97.92%、97.92%、95.83%。相对标准偏差(relative standard deviation, RSD, n=6)为2.12%~12.28%。结论 该方法基本能够满足应用于实际样品的分析检测, 较传统检测方法更加简便快捷, 使用试剂少, 灵敏度高。

英文摘要:

      Objective To establish a method for the determination of 48 kinds of pesticides residues in eggs by QuEChERS pretreatment and gas chromatography-tandem mass spectrometry. Methods The sample was dehydrated and extracted with 1% acetonitrile acetate, MgSO4 and NaOAC mixed salt package, and purified by MgSO4, PSA, GCB and C18 mixed purification tube. The purified solution was concentrated by nitrogen blowing and then the volume of ethyl acetate was determined. The sample was separated by gas chromatography, determined by MRM mode, corrected by internal standard and quantified by external standard method. Results The linear range of 48 pesticides was 5–100 ng/mL, and the r2 was above 0.995. The detection limit of the method was 0.03–5.00 μg/kg, and the quantitative limit of the method was 0.12–17.00 μg/kg. The average recoveries of 48 pesticides at 3 levels of 5, 10 and 50 μg/kg in the range of 70%–120% were 97.92%, 97.92% and 95.83%, respectively. The relative standard deviation (relative standard deviation, RSD, n=6) was 2.12%–12.28%. Conclusion This method can be applied to the analysis and detection of actual samples. It is more convenient and quick than the traditional method, and has less reagents and high sensitivity.