Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo 1, Tarragona 43007, Spain.
Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo 1, Tarragona 43007, Spain.
J Chromatogr A. 2022 Aug 2;1676:463237. doi: 10.1016/j.chroma.2022.463237. Epub 2022 Jun 12.
Four novel mixed-mode zwitterionic silica-based functionalized with strong moieties sorbents were synthesized and evaluated through solid-phase extraction (SPE) to determine acidic and basic drugs in environmental water samples. All sorbents had the same functionalization: quaternary amine and sulfonic groups and C chains so that hydrophobic and strong cationic exchange (SCX) and strong anionic exchange (SAX) interactions could be exploited, in addition, two of them had carbon microparticles embedded. All sorbents retained both acidic and basic compounds in the preliminary assays but only the basic compounds were retained selectively through ionic exchange interactions when a clean-up step was introduced. The SPE method was therefore optimized to promote the selective retention of the basic compounds, initially with the two best-performing sorbents. After optimization of the SPE protocol, these sorbents were evaluated for the analysis of environmental water samples using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method with the best-performing sorbent was then validated with 100 mL of river samples and 50 mL of effluent wastewater samples in terms of apparent recoveries (%R) spiking samples at 50 ng/L (river) and 200 ng/L (river and effluent), matrix effect, linear range, method quantification and detection limits, repeatability, and reproducibility. It should be highlighted that %R ranged from 40 to 85% and matrix effects ranged from -17 to -4% for spiked river samples. When the method was applied to river and effluent wastewater samples, most compounds were found in the range from 24 to 1233 ng/L with detection limits from 1 to 5 ng/L.
四种新型混合模式两性离子硅胶基功能化强基团吸附剂被合成并通过固相萃取（SPE）进行评价，以测定环境水样中的酸性和碱性药物。所有的吸附剂都有相同的官能化：季铵和磺酸基团和 C 链，以便可以利用疏水性和强阳离子交换（SCX）和强阴离子交换（SAX）相互作用，此外，其中两种具有嵌入的碳微粒。所有的吸附剂在初步试验中都保留了酸性和碱性化合物，但只有当引入清洗步骤时，通过离子交换相互作用才能选择性地保留碱性化合物。因此，SPE 方法进行了优化，以促进碱性化合物的选择性保留，最初使用两种性能最佳的吸附剂。在优化 SPE 方案后，使用液相色谱-串联质谱（LC-MS/MS）对这些吸附剂进行了环境水样分析的评估。然后，使用性能最佳的吸附剂，通过在 50ng/L（河流）和 200ng/L（河流和废水）的浓度下对 100mL 河水样品和 50mL 废水样品进行加标，对该方法进行了验证，从 50ng/L（河流）和 200ng/L（河流和废水）的浓度下对 100mL 河水样品和 50mL 废水样品进行加标，评估了该方法的表观回收率（%R）、基质效应、线性范围、方法定量和检测限、重复性和重现性。值得强调的是，加标河水样品的%R 范围为 40%至 85%，基质效应范围为-17%至-4%。当该方法应用于河水和废水样品时，大多数化合物的浓度范围为 24 至 1233ng/L，检测限为 1 至 5ng/L。
