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

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

关键词:  ,静电轨道阱质谱,正负切换,农药残留化合物,同时筛查和定量

Key words:  orbitrap mass spectrometry  positive and negative switching mode  pesticides residue  synchronous screening and quantitation  

摘要:

建立了超高效液相色谱-静电轨道阱质谱法检测饲料中的51种农药残留物的检测方法和目标化合物的质谱数据库。饲料样品经0.1 mol/mL HCl : 甲醇=1:3提取,高速离心,经稀释后进样分析。采用Thermo Syncronis C18色谱柱(150 mm×2.1 mm, 3 μm)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种农药残留化合物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,适用于饲料中同时筛查和定量农药残留化合物。

Abstract:

To screen and quantify 51 pesticides residue in feed synchronously, an ultra performance liquid chromatography-orbitrap mass spectrometry method and the target compounds data base were established. Feed was extracted by 0.1 mol/mL HCl : menthanol =1:3. The extraction was high speed centrifuged and purified by acid then diluted to inject. Thermo Syncronis C18 column (150 mm×2.1 mm, 3 μm) was chosen to be the solid phase and 0.1 % formic acid combined with 0.1 % formic acid acetonitrile were chosen to be the liquid phase to 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 ion was used to achieve the quantitation. Under the optimal conditions, 51 pesticides were separated well, Good linearity was obtained in their respective quantitative range (correlation coefficients r≥0.99 ). The average recoveries were in the range of 50.61 ％～ 109.49 % and the relative standard deviations (RSD) were lower than 9.1%. The method was proved to be convenient, economical, sensitive and accurate. The research was proved to be effective for the screening and quantitation of 51 pesticides residue in feed.