Laboratorios Cavendish S.L. Research Department, E-18220 Granada, Spain.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2010 Nov;27(11):1532-44. doi: 10.1080/19440049.2010.506602.
A rapid, simple and sensitive multi-residue method was developed and validated for the simultaneous quantification and confirmation of 69 pesticides in fruit and vegetables using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted following the quick, easy, cheap, effective, rugged and safe method known as QuEChERS. Mass spectrometric conditions were individually optimised for each analyte in order to achieve maximum sensitivity in multiple reaction monitoring (MRM) mode. Using the developed chromatographic conditions, 69 pesticides can be separated in less than 17 min. Two selected reaction monitoring (SRM) assays were used for each pesticide to obtain simultaneous quantification and identification in one run. With this method in SRM mode, more than 150 pesticides can be analysed and quantified, but their confirmation is not possible in all cases according to the European regulations on pesticide residues. Nine common representative matrices (zucchini, melon, cucumber, watermelon, tomato, garlic, eggplant, lettuce and pepper) were selected to investigate the effect of different matrices on recovery and precision. Mean recoveries ranged from 70% to 120%, with relative standard deviations (RSDs) lower than 20% for all the pesticides. The proposed method was applied to the analysis of more than 2000 vegetable samples from the extensive greenhouse cultivation in the province of Almeria, Spain, during one year. The methodology combines the advantages of both QuEChERS and LC-MS/MS producing a very rapid, sensitive, accurate and reliable procedure that can be applied in routine analytical laboratories. The method was validated and accredited according to UNE-EN-ISO/IEC 17025:2005 international standard (accreditation number 278/LE1027).
建立并验证了一种快速、简单、灵敏的多残留分析方法，采用液相色谱-串联质谱（LC-MS/MS）技术，同时对果蔬中 69 种农药进行定量和确证分析。样品采用 QuEChERS 方法提取，该方法具有快速、简便、廉价、有效、耐用和安全的特点。为了在多反应监测（MRM）模式下达到最大灵敏度，对每种分析物的质谱条件进行了单独优化。采用所建立的色谱条件，可在 17 分钟内分离 69 种农药。每种农药均采用两种选择反应监测（SRM）方法进行同时定量和确证分析。采用该方法的 SRM 模式，可以分析和定量 150 多种农药，但根据欧洲农药残留法规，并非所有情况下都可以进行确证。选择了 9 种常见的代表性基质（西葫芦、甜瓜、黄瓜、西瓜、番茄、大蒜、茄子、生菜和辣椒），以考察不同基质对回收率和精密度的影响。所有农药的平均回收率在 70%至 120%之间，相对标准偏差（RSD）均低于 20%。该方法应用于西班牙阿尔梅里亚省大规模温室种植的 2000 多个蔬菜样品分析，每年进行一次。该方法结合了 QuEChERS 和 LC-MS/MS 的优点，具有快速、灵敏、准确、可靠的特点，可应用于常规分析实验室。该方法按照 UNE-EN-ISO/IEC 17025:2005 国际标准进行了验证和认可（认可编号 278/LE1027）。
