Institute of Chemistry, Saint-Petersburg University St.Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab, St. Petersburg, 199034, Russia.
Institute of Chemistry, Saint-Petersburg University St.Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab, St. Petersburg, 199034, Russia.
Talanta. 2020 Mar 1;209:120587. doi: 10.1016/j.talanta.2019.120587. Epub 2019 Nov 24.
A fully automated in-syringe switchable hydrophilicity solvent-based microextraction approach was suggested for the first time. Di-(2-ethylhexyl)phosphoric acid was investigated as a novel switchable hydrophilicity solvent. The microextraction procedure implemented into a syringe pump included dissociation of the extractant in alkaline sample solution resulting in homogeneous solution formation followed by in situ organic phase generation by acidification and its separation. The microextraction procedure was applied to the HPLC-UV determination of antimicrobial drugs (sulfamethoxazole and sulfamethazine) in human urine samples as a proof-of-concept example. The calibration graphs were linear over the concentration ranges of 0.06-50 mg L for sulfamethoxazole and 0.13-50 mg L for sulfamethazine. The LODs calculated from the blank tests based on 3σ were 0.02 and 0.04 mg L for sulfamethoxazole and sulfamethazine, respectively. The sample throughput was 12 samples h. The possibility of using the proposed procedure for assessing sulfamethoxazole/sulfamethazine acetylation in metabolic processes by individual human phenotypes was shown.
首次提出了一种全自动化注射器内可切换亲水性溶剂的微萃取方法。二(2-乙基己基)磷酸被研究为一种新型可切换亲水性溶剂。该微萃取程序通过在碱性样品溶液中使萃取剂离解，形成均相溶液，然后通过酸化原位生成有机相并将其分离来实现。该微萃取程序被应用于 HPLC-UV 测定人尿样中的抗菌药物（磺胺甲恶唑和磺胺甲嘧啶），作为概念验证实例。对于磺胺甲恶唑，校准曲线在 0.06-50mg/L 的浓度范围内呈线性，对于磺胺甲嘧啶，校准曲线在 0.13-50mg/L 的浓度范围内呈线性。基于 3σ 计算的空白测试的 LOD 分别为 0.02 和 0.04mg/L，用于磺胺甲恶唑和磺胺甲嘧啶。样品通量为 12 个样品/h。结果表明，该方法可用于评估个体人类表型代谢过程中磺胺甲恶唑/磺胺甲嘧啶的乙酰化作用。
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