基于浮相有机液滴固化的空气辅助液-液微萃取法，通过化学计量学方法，同时萃取和分光光度法测定生物样品中的一些药物。
Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods.
机构信息
Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51644-14766, Iran.
Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51644-14766, Iran.
出版信息
Spectrochim Acta A Mol Biomol Spectrosc. 2018 Jan 5;188:72-79. doi: 10.1016/j.saa.2017.06.069. Epub 2017 Jul 3.
An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40μg mL for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08μg mL for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.
一种基于空气辅助的液-液微萃取方法，采用固-液分散萃取（SFOD）方法，结合多元校正方法，即偏最小二乘法（PLS），通过分光光度法快速、简便地测定生物样品中的阿替洛尔（ATE）、普萘洛尔（PRO）和卡维地洛（CAR）。该方法将中性水溶液中的分析物萃取到 1-十二醇作为有机溶剂中，采用 AALLME 萃取。在这种方法中，使用接近室温的低熔点溶剂作为萃取溶剂。通过 10ml 玻璃注射器反复吸入和推出水相样品溶液和萃取溶剂混合物 10 次，立即形成乳状液。离心后，通过将乳液在低于熔点的温度下固化，可简单地从水相中收集萃取剂液滴。在下一个步骤中，同时将分析物反萃取到酸性水溶液中。德林格和苏伊奇多响应优化用于同时优化三个分析物的参数。该方法结合了空气辅助液-液微萃取（AALLME）和分散液-液微萃取（DLLME-SFOD）的优点，考虑了浮油性有机液滴的固化。在优化条件下，ATE、CAR 和 PRO 的校准曲线在 0.30-6.00、0.32-2.00 和 0.30-1.40μgml 范围内呈线性。获得了其他分析参数如下：富集因子（EFs）分别为 11.24、16.55 和 14.90，检测限（LODs）分别为 0.09、0.10 和 0.08μgml 用于 ATE、CAR 和 PRO。该方法在应用过程中既不需要用于萃取的高毒性氯化溶剂，也不需要有机溶剂分散剂，因此更加环保。
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