Department of Instrumental Analysis, Faculty of Pharmacy, University of Concepcion, PO Box 160-C, Concepcion, Chile; Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1, Canada.
Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1, Canada.
Talanta. 2020 May 1;211:120714. doi: 10.1016/j.talanta.2020.120714. Epub 2020 Jan 7.
A semi-automated and sensitive method was developed for simultaneous determination of the six most consumed artificial sweeteners (AS) in surface waters using thin-film solid-phase microextraction (TF-SPME) and high-performance liquid chromatography (HPLC). A triple quadrupole mass spectrometer and an electrospray ionization source (ESI-MS) run in negative ionization and multiple reaction monitoring modes were employed for instrumental analysis. The TF-SPME method was optimized for the extraction phase, sample pH, desorption solvent, extraction time, and desorption time. In-house-synthetized-hydrophilic-lipophilic balance weak anion exchange (HLB-WAX) particles imbedded within a polyacrylonitrile (PAN) binder were selected as the extraction phase for the thin-film coating due to their cost-effectiveness and enhanced sensitivity for artificial sweeteners. Suitable analytical parameters that include linearity (R > 0.9914), recovery > 80%, inter, and intra-reproducibility less than 18% were obtained for the AS compounds studied. The developed method estimated limits of detection (LODs) ranging from 0.004 to 0.038 ng mL The SPME method was successfully applied for the determination of ultra-trace levels of AS in water samples collected from Grand River (Ontario, Canada), downstream of three municipal wastewater treatment plants (WWTPs). Concentrations ranging from 0.03 to 20.3 ng mL were found for the AS compounds studied.
一种半自动化和灵敏的方法已被开发出来，用于使用薄膜固相微萃取（TF-SPME）和高效液相色谱（HPLC）同时测定地表水中的六种最常消耗的人工甜味剂（AS）。三重四极杆质谱仪和电喷雾电离源（ESI-MS）以负离子和多反应监测模式运行，用于仪器分析。TF-SPME 方法针对萃取相、样品 pH 值、解吸溶剂、萃取时间和解吸时间进行了优化。由于成本效益高且对人工甜味剂的灵敏度增强，因此选择内合成的亲脂性平衡弱阴离子交换（HLB-WAX）颗粒嵌入到聚丙烯腈（PAN）粘结剂中作为薄膜涂层的萃取相。对于所研究的 AS 化合物，获得了合适的分析参数，包括线性（R > 0.9914）、回收率> 80%、日内和日间重现性小于 18%。开发的方法估计检测限（LOD）范围为 0.004 至 0.038 ng mL-1。SPME 方法成功应用于测定从安大略省格兰德河（加拿大）采集的水样中的超痕量 AS，这些水样来自三个市政污水处理厂（WWTP）的下游。在所研究的 AS 化合物中发现浓度范围为 0.03 至 20.3 ng mL-1。
