超高效液相色谱-静电轨道阱质谱正负切换同时筛查定量谷物饲料中的51种农药残留

Synchronous Screening and Quantitation of 51 Pesticides Residue in Grain Feed by Ultra Performance Liquid Chromatography-Orbitrap Mass Spectrometry with Positive and Negative Switching Mode

建立了超高效液相色谱-静电轨道阱质谱法检测谷物饲料中的51种农药残留物的检测方法和目标化合物的质谱数据库。谷物饲料样品经0.1 mol/m L HCl∶甲醇=1∶3提取,高速离心,稀释后进样分析。采用Thermo Syncronis C18色谱柱(150 mm×2.1 mm,3μm)作为固定相,0.1%甲酸和0.1%甲酸乙腈作为流动相进行梯度洗脱。质谱采用正负切换离子扫描,一对母离子和子离子的精确质量数进行定性,以母离子的响应强度积分面积进行定量分析。51种农药残留在最优化条件下分离良好,在定量范围内均线性良好(线性相关系数r≥0.99),回收率也可达到50.61%~109.49%,相对标准偏差(RSD)小于9.1%。本方法具有简便、快速、灵敏、准确等特点,适用于谷物饲料中同时筛查和定量农药残留化合物。

To screen and quantify 51 pesticides residue in grain feed synchronously, an ultra performance liquidchromatography-orbitrap mass spectrometry method and the target compounds data base were established. Grainfeed was extracted by 0.1 mol/ mL HCl ： menthanol =1：3. The extraction was high speed centrifuged and purifiedby acid then diluted to inject. Thermo Syncronis C18 column （150 mm×2.1 mm, 3 μm） was chosen to be thesolid phase and 0.1% formic acid combined with 0.1% formic acid acetonitrile were chosen to be the liquid phaseto achieve the grad elution. The mass spectrometer was operated using positive and negative switching scan mode.One pair of parent ion and daughter ion were chosen to achieve the qualitation and the response of the parent ionwas used to achieve the quantitation. Under the optimal conditions, 51 pesticides were separated well, Goodlinearity was obtained in their respective quantitative range （correlation coefficients r ≥0. 99）. The averagerecoveries were in the range of 50.61% ～109.49% and the relative standard deviations （RSD） were lower than9.1%. The method was proved to be convenient, economical, sensitive and accurate. The research was proved tobe effective for the screening and quantitation of 51 pesticides residue in grain feed.