基于QuEChERS-气相色谱-串联质谱法测定鸡蛋中48种农药残留

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0.03～5.00μg/kg之间,方法定量限在0.12～17.00μg/kg之间。48种农药在5、10和50μg/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。

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

ABSTRACT: Objective To determination of 48 kinds of pesticides residues by using the QuEChERS in eggs by gas chromatography-tandem mass spectrometry(GC-MS/MS) . Methods The sample was extracted by dehydration with 1% acetonitril eacetate?, MgSO4 and NaOAC mixed salt package,purified by a mixed purification tube containing MaSO4,PSA ,GCB and C18.The purification solution was concentrated by nitrogen blowing and then ethyl acetate was fixed volume, separated on Gas chromatography,followed by the measurement of MRM mode, and internal standard was corrected, external standard method are quantified simultaneously Results The relationship of 48 pesticides was good within the linear range of 5~100ng/mL, and all R2 was above 0.995. The limit of detection(LOD)was 0.03~5.00ug/kg, and the limit of quantitation(LOQ )was 0.12~17.00ug/kg.The average recoveries rates of 70%-120% were 97.92%, 97.92% and 95.83% respectively for 48 pesticides at 5, 10 and 50ug/kg . The relative standard deviation(RSD,n=6) range from 2.12% to 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, has less reagents and high sensitivity., which provides detection of pesticide residues in eggs.