Département de Chimie, Université de Montréal, Pavillon Roger-Gaudry, 2900 Edouard-Montpetit, Montréal, Québec, H3C 3J7, Canada.
GRIL, Département de Sciences Biologiques, Université de Montréal, Pavillon Marie-Victorin 90, Avenue Vincent-d'Indy, Montréal, Québec, H2V 2S9, Canada.
Anal Bioanal Chem. 2018 Apr;410(11):2765-2779. doi: 10.1007/s00216-018-0957-2. Epub 2018 Mar 5.
A study was initiated to investigate a fast and reliable method for the determination of selected systemic insecticides in water matrixes and to evaluate potential sources of bias in their analysis. Acetamiprid, clothianidin, desnitro-imidacloprid, dinotefuran, fipronil, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam were amenable to analysis via on-line sample enrichment hyphenated to ultra-high-performance liquid chromatography tandem mass spectrometry. The selection of on-line solid-phase extraction parameters was dictated by a multicriterion desirability approach. A 2-mL on-line injection volume with a 1500 μL min loading flow rate met the objectives sought in terms of chromatographic requirements, extraction efficiency, sensitivity, and precision. A total analysis time of 8 min per sample was obtained with method limits of detection in the range of 0.1-5 ng L for the scope of targeted analytes. Automation at the sample concentration step yielded intraday and interday precisions in the range of 1-23 and 2-26%, respectively. Factors that could affect the whole method accuracy were further evaluated in matrix-specific experiments. The impact of the initial filtration step on analyte recovery was evaluated in ultra-pure water, tap water, and surface water. Out of the nine membranes tested, glass fiber filters and polyester filters appeared as the most appropriate materials. Sample storage stability was also investigated across the three matrix types; the targeted analytes displayed suitable stability during 28 days at either 4 °C or - 20 °C, with little deviations (± 10%) with respect to the initial T concentration. Method applicability was demonstrated in a range of tap water and surface water samples from the province of Québec, Canada. Results from the present survey indicated a predominance of thiamethoxam (< 0.5-10 and 3-61 ng L in tap water and river water, respectively), clothianidin (< 0.5-6 and 2-88 ng L in tap water and river water, respectively), and imidacloprid (< 0.1-1 and 0.8-38 ng L in tap water and river water, respectively) among the targeted analytes. Graphical abstract ᅟ Development of solid-phase extraction coupled on-line to UHPLC-MS/MS for the rapid screening of systemic insecticides in water.
发起了一项研究，旨在开发一种快速可靠的方法，用于测定水基质中选定的系统杀虫剂，并评估其分析中潜在的偏倚来源。乙虫腈、噻虫嗪、噻虫啉、呋虫胺、氟虫腈、吡虫啉、涕灭威、噻虫胺和噻虫砜可通过在线样品富集与超高效液相色谱串联质谱联用进行分析。在线固相萃取参数的选择取决于多准则理想性方法。2 毫升在线进样体积和 1500μL/min 的加载流速满足了色谱要求、萃取效率、灵敏度和精密度方面的目标。每个样品的总分析时间为 8 分钟，目标分析物的方法检出限范围为 0.1-5ng/L。在样品浓缩步骤实现自动化，可得到日内和日间精密度分别为 1-23%和 2-26%。进一步在基质特异性实验中评估了可能影响整个方法准确性的因素。在超纯水、自来水和地表水三种基质中评估了初始过滤步骤对分析物回收率的影响。在所测试的九种膜中，玻璃纤维过滤器和聚酯过滤器似乎是最合适的材料。还研究了三种基质类型中的样品储存稳定性；目标分析物在 4°C 或-20°C 下储存 28 天，与初始 T 浓度相比，只有很小的偏差（±10%），表现出良好的稳定性。该方法在加拿大魁北克省的自来水和地表水样本中得到了验证。本调查结果表明，噻虫嗪（自来水中<0.5-10 和 3-61ng/L，河水中<0.5-6 和 2-88ng/L）、噻虫胺（自来水中<0.5-6 和 2-88ng/L，河水中<0.5-6 和 2-88ng/L）和吡虫啉（自来水中<0.1-1 和 0.8-38ng/L，河水中<0.1-1 和 0.8-38ng/L）是目标分析物中的主要成分。
