Requimte, Instituto Superior de Engenharia, Instituto Politécnico do Porto, Rua Dr António Bernardino de Almeida, 431, 4200-072, Porto, Portugal.
J Am Soc Mass Spectrom. 2012 Dec;23(12):2187-97. doi: 10.1007/s13361-012-0488-6. Epub 2012 Sep 20.
Multiclass analysis method was optimized in order to analyze pesticides traces by gas chromatography with ion-trap and tandem mass spectrometry (GC-MS/MS). The influence of some analytical parameters on pesticide signal response was explored. Five ion trap mass spectrometry (IT-MS) operating parameters, including isolation time (IT), excitation voltage (EV), excitation time (ET), maximum excitation energy or "q" value (q), and isolation mass window (IMW) were numerically tested in order to maximize the instrument analytical signal response. For this, multiple linear regression was used in data analysis to evaluate the influence of the five parameters on the analytical response in the ion trap mass spectrometer and to predict its response. The assessment of the five parameters based on the regression equations substantially increased the sensitivity of IT-MS/MS in the MS/MS mode. The results obtained show that for most of the pesticides, these parameters have a strong influence on both signal response and detection limit. Using the optimized method, a multiclass pesticide analysis was performed for 46 pesticides in a strawberry matrix. Levels higher than the limit established for strawberries by the European Union were found in some samples.
为了通过气相色谱-离子阱串联质谱法(GC-MS/MS)分析农药痕迹,优化了多类别分析方法。研究了一些分析参数对农药信号响应的影响。数值测试了五种离子阱质谱(IT-MS)操作参数,包括隔离时间(IT)、激发电压(EV)、激发时间(ET)、最大激发能量或“q”值(q)和隔离质量窗口(IMW),以最大化仪器分析信号响应。为此,在数据分析中使用了多元线性回归来评估这五个参数对离子阱质谱仪中分析响应的影响,并预测其响应。基于回归方程对五个参数的评估极大地提高了 IT-MS/MS 在 MS/MS 模式下的灵敏度。结果表明,对于大多数农药,这些参数对信号响应和检测限都有很强的影响。使用优化的方法,在草莓基质中对 46 种农药进行了多类别分析。在一些样本中发现,某些农药的浓度高于欧盟为草莓设定的限量。