Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Jaén, Spain.
Talanta. 2010 Jun 15;81(4-5):1310-21. doi: 10.1016/j.talanta.2010.02.026. Epub 2010 Feb 13.
This work reports a rapid and reliable method for the determination of 33 multi-class pesticides in fruit-based soft drinks. The proposed method consists of a sample treatment step based on solid-phase extraction using hydrophilic-lipophilic balanced polymer-based reverse-phase SPE cartridges, followed by identification and quantitation of the target pesticides by rapid resolution liquid chromatography using a short C(18) column (4.6mm x 50mm) with 1.8microm particle size and mass spectrometric detection using electrospray time-of-flight mass spectrometry (LC-TOFMS). The identification and confirmation of the compounds were based on retention time matching along with the accurate mass measurements of the protonated molecules (M+H) and their main fragment ions. Fruit-based soft drinks spiked at different fortification levels (10 and 50microgL(-1)) yielded average recoveries in the range 66-124% with RSD (%) below 14% (n=6). The obtained limits of quantitation varied in the range 0.02-2microgL(-1). The proposed method was successfully applied to the analysis of 14 market-purchased fruit-based soft drinks samples collected in some European countries, showing its potential applicability and revealing the presence of some of the target species in the microgL(-1) range.
本工作报道了一种快速可靠的方法，用于测定水果软饮料中的 33 种多类农药。该方法包括固相萃取样品处理步骤，采用亲水亲脂平衡聚合物反相 SPE 小柱，然后通过短 C（18）柱（4.6mm x 50mm）和质量色谱法进行快速分辨液相色谱分析，粒径为 1.8μm，采用电喷雾飞行时间质谱（LC-TOFMS）进行质谱检测。化合物的鉴定和确证基于保留时间匹配以及质子化分子（[M+H]（+））及其主要碎片离子的精确质量测量。在不同浓度水平（10 和 50μg/L）下，水果软饮料的平均回收率在 66-124%之间，相对标准偏差（RSD）%低于 14%（n=6）。定量下限在 0.02-2μg/L 范围内变化。该方法成功应用于分析在一些欧洲国家购买的 14 个市售水果软饮料样品，显示出其潜在的适用性，并揭示了一些目标物质在微gL（-1）范围内的存在。
