González-Rodríguez M J, Garrido-Frenich A, Arrebola F J, Martínez-Vidal J L
Department of Analytical Chemistry, University of Almería, 04120 Almería, Spain.
Rapid Commun Mass Spectrom. 2002;16(12):1216-24. doi: 10.1002/rcm.707.
A rapid multiresidue method for the analysis of 72 pesticides has been developed using a single injection with low-pressure gas chromatography/tandem mass spectrometry (LP-GC/MS/MS). The LP-GC/MS/MS method used a short capillary column of 10 m x 0.53 mm i.d. x 0.25 microm film thickness coupled with a 0.6 m x 0.10 mm i.d. restriction at the inlet end. Optimal LP-GC conditions were determined which achieved the fastest separation in MS/MS detection mode. Also MS/MS conditions were optimized in order to increase sensitivity and selectivity. The analytical parameters of the LP-GC/MS/MS method were compared with those obtained by GC/MS/MS using a conventional capillary column (30 m x 0.25 mm i.d. x 0.25 microm film thickness). Better precision and sensitivity values were obtained with the LP-GC/MS/MS approach. The limits of detection (LOD) of the compounds ranged from 0.1 to 14.1 microg L(-1) for LP-GC/MS/MS, lower than those obtained for conventional GC/MS/MS that ranged from 0.1 to 17.5 microg L(-1). The peak widths obtained with the short column in LP-GC are similar to those obtained using conventional capillary GC columns, and the peaks can be successfully identified by MS/MS detection with the conventional scan speed of ion-trap instruments. In addition, the analysis time was significantly reduced with LP-GC/MS/MS (32 min) versus GC/MS/MS (72 min), allowing the number of samples analyzed per day in a routine laboratory to be doubled.
已开发出一种快速多残留方法,用于分析72种农药,该方法采用单次进样的低压气相色谱/串联质谱法(LP-GC/MS/MS)。LP-GC/MS/MS方法使用一根10 m×0.53 mm内径×0.25μm膜厚的短毛细管柱,并在进样端连接一根0.6 m×0.10 mm内径的限流管。确定了最佳的LP-GC条件,在MS/MS检测模式下实现了最快的分离。同时优化了MS/MS条件以提高灵敏度和选择性。将LP-GC/MS/MS方法的分析参数与使用常规毛细管柱(30 m×0.25 mm内径×0.25μm膜厚)的GC/MS/MS所获得的参数进行了比较。LP-GC/MS/MS方法获得了更好的精密度和灵敏度值。LP-GC/MS/MS对化合物的检测限(LOD)范围为0.1至14.1μg L⁻¹,低于常规GC/MS/MS的检测限(范围为0.1至17.5μg L⁻¹)。LP-GC中短柱获得的峰宽与使用常规毛细管GC柱获得的峰宽相似,并且可以通过离子阱仪器的常规扫描速度,利用MS/MS检测成功鉴定这些峰。此外,与GC/MS/MS(72分钟)相比,LP-GC/MS/MS(32分钟)的分析时间显著缩短,使常规实验室每天能够分析的样品数量增加一倍。