Martínez Vidal J L, Arrebola F J, Mateu-Sánchez M
Department of Analytical Chemistry, University of Almería, 04071 Almería, Spain.
Rapid Commun Mass Spectrom. 2002;16(11):1106-15. doi: 10.1002/rcm.686.
The use of gas chromatography/tandem mass spectrometry (GC/MS/MS) applied to determine multiple pesticide residues in fresh vegetables has been thoroughly studied. A single injection method to detect, confirm and quantify 54 multiclass pesticides has been developed and applied in a routine analysis laboratory. The proposed method consists of a rapid extraction of 15 g of vegetable sample with dichloromethane. An additional clean-up step is not necessary even when injecting 10 microL of extract. Instead the gas chromatograph was fitted with a carbofrit inserted into the glass liner and a guard column. In addition, the detection mode chosen (MS/MS) provides additional selectivity. The method has been validated and applied to 1300 samples in a routine laboratory following specified quality criteria. The recovery efficiencies obtained for all the pesticides ranged between 70.2 and 110.8% at two different fortification levels. The relative standard deviation for quantification (RSD) was lower than 16.7% for all the compounds. Important experimental parameters, such as the conditioning of carbofrit, overload of the analytical column, and cleanliness of the ion trap, were evaluated for their influence on the performance of the method.
气相色谱/串联质谱法(GC/MS/MS)用于测定新鲜蔬菜中多种农药残留的研究已十分深入。一种单次进样检测、确证和定量54种多类农药的方法已被开发出来并应用于常规分析实验室。该方法包括用二氯甲烷对15克蔬菜样品进行快速萃取。即使进样10微升萃取液,也无需额外的净化步骤。相反,气相色谱仪配备了插入玻璃衬管的碳滤片和保护柱。此外,所选择的检测模式(MS/MS)提供了额外的选择性。该方法已按照规定的质量标准在常规实验室中进行了验证,并应用于1300个样品。在两个不同的加标水平下,所有农药的回收率在70.2%至110.8%之间。所有化合物的定量相对标准偏差(RSD)均低于16.7%。对重要的实验参数,如碳滤片的预处理、分析柱的过载以及离子阱的清洁情况,评估了它们对方法性能的影响。