Department of Analytical Chemistry, Faculty of Chemistry, University of Seville, c/Prof. García González s/n, 41012, Seville, Spain; Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
Department of Analytical Chemistry, Universitat Autónoma de Barcelona, 08193 Bellaterra, Barcelona, Spain.
J Chromatogr A. 2021 Aug 30;1652:462344. doi: 10.1016/j.chroma.2021.462344. Epub 2021 Jun 15.
Liquid phase microextraction (LPME) into a microfluidic has undergone great advances focused on downscaled and miniaturized devices. In this work, a microfluidic device was developed for the extraction of sulfonamides in order to accelerate the mass transfer and passive diffusion of the analytes from the donor phase to the acceptor phase. The subsequent analysis was carried out by high performance liquid chromatography with UV-DAD (HPLC-DAD). Several parameters affecting the extraction efficiency of the method such as the supported liquid membrane, composition of donor and acceptor phase and flow rate were investigated and optimized. Tributyl phosphate was found to be a good supported liquid membrane which confers not only great affinity for analytes but also long-term stability, allowing more than 20 consecutive extractions without carry over effect. Under optimum conditions, extraction efficiencies were over 96 % for all sulfonamides after 10 minutes extraction and only 10 µL of sample was required. Relative standard deviation was between 3-5 % for all compounds. Method detection limits were 45, 57, 54 and 33 ng mL for sulfadiazine (SDI), sulfamerazine (SMR), sulfamethazine (SMT) and sulfamethoxazole (SMX), respectively. Quantitation limits were 0.15, 0.19, 0.18 and 0.11 µg mL for SDI, SMR, SMT SMX, respectively. The proposed microfluidic device was successfully applied for the determination of sulfonamides in urine samples with extraction efficiencies within the range of 86-106 %. The proposed method improves the procedures proposed to date for the determination of sulfonamides in terms of efficiency, reduction of the sample volume and extraction time.
液相微萃取（LPME）进入微流控技术领域取得了重大进展，重点是缩小和微型化设备。在这项工作中，开发了一种微流控装置，用于从供体相到受体相加速分析物的传质和被动扩散，以萃取磺胺类药物。随后的分析通过高效液相色谱与紫外可见（HPLC-DAD）进行。考察并优化了影响方法萃取效率的几个参数，如支撑液膜、供体相和受体相的组成和流速。发现磷酸三丁酯是一种良好的支撑液膜，它不仅对分析物具有很大的亲和力，而且具有长期稳定性，允许进行 20 多次连续萃取而没有夹带效应。在最佳条件下，所有磺胺类药物在 10 分钟萃取后萃取效率均超过 96％，仅需 10µL 样品。所有化合物的相对标准偏差在 3-5％之间。磺胺嘧啶（SDI）、磺胺甲噁唑（SMR）、磺胺甲嘧啶（SMT）和磺胺甲噁唑（SMX）的方法检测限分别为 45、57、54 和 33ngmL。磺胺嘧啶（SDI）、磺胺甲噁唑（SMR）、磺胺甲嘧啶（SMT）和磺胺甲噁唑（SMX）的定量限分别为 0.15、0.19、0.18 和 0.11µgmL。该微流控装置成功应用于尿液样品中磺胺类药物的测定，萃取效率在 86-106％范围内。与迄今为止提出的磺胺类药物测定方法相比，该方法在效率、减少样品体积和萃取时间方面有所改进。
