气相色谱法/三重四极杆质谱测定番茄酱中72种农药残留量

Determination of 72 Pesticide Residues in Tomato Paste by TSQ QUANTUMN-GC

采用气相色谱法/三重四极杆质谱分析技术,通过全扫描、子离子扫描和选择离子扫描,确定甲胺磷等72种农药二级质谱分析时适用的标准工作液质量浓度、SRM监测离子对、质谱采集时间窗口,以及碰撞能量等质谱参数;与QueChers样品前处理方法结合,开发出了番茄酱中多农残快速检测的气相色谱-质谱/质谱分析方法。方法表明:在线性范围5～2000μg/L内,72种农药的线性相关系数均大于0.99;3个水平的添加回收实验结果表明,低水平的加标条件下95.8%的农药回收率为80%～120%,87.5%的农药相对标准偏差(RSD)小于15%;检出限(RSN=3)和定量限(RSN=10)分别为0.04～7.5μg/kg和0.1～12.9μg/kg。该方法灵敏度高、实现了低含量的定量分析、准确可靠,满足农药残留分析的要求。

A novel method was developed for the determination of 72 pesticide residues in tomato paste by TSQ QUANTUMN GC （GC-MS/MS） combined with QueChers extraction. Optimal concentrations of standard working solutions, SEM （selected ion monitoring） ion pairs, acquisition time window and collision energy were established for MS/ MS analysis of methamidophos and 71 other pesticides in full scan, daughter ion scan and selected ion scan modes. Over the linear range of 5 to 2000 μg/L, the correlation coefficient for each pesticide was bigger than 0.99. Recoveries from spiked samples at three levels indicated that 95.8% of the tested pesticides exhibited a recovery range of 80% to 120% with relative standard deviation smaller than 15% for 87.5% of them. The limits of detection （RsN = 3） varied over the range of 0.04 to 7.5 μg/kg, and limits of quantification （RSN = 10） ranged from 0.1 to 12.9 μg/kg. This method could provide a sensitive, accurate and reilable approach that meets the requirments for quantitative analysis of low levels of pesticides.