Rahimi Atyeh, Nojavan Saeed, Tabani Hadi
Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., Evin, Tehran 1983963113, Iran.
Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., Evin, Tehran 1983963113, Iran.
J Pharm Biomed Anal. 2020 May 30;184:113175. doi: 10.1016/j.jpba.2020.113175. Epub 2020 Feb 14.
In this work, a new mode of gel-electromembrane extraction (G-EME), called "inside" gel-EME (IG-EME) is proposed for the extraction of morphine and codeine as model basic drugs from complex biological samples. Here, an aqueous media that was captured inside the agarose gel membrane, acted as both gel membrane and the acceptor phase (AP) at the same time. In this regard, the membrane served as the separation filter (membrane) and supported liquid acceptor phase (SLAP) as well. With this new development, unwanted changes of the AP volume during the extraction, which is a common issue in the G-EME (due to electroendosmosis (EEO) phenomenon), was addressed properly. Briefly, the setup involved insertion of negative electrode inside the gel membrane and positive electrode into the donor phase (DP). Following that, the IG-EME was easily performed using optimal conditions (pH of the DP: 6.0; membrane composition (agarose concentration: 1% (w/v) in aqueous media with pH 3.0, and 15 mm thickness); voltage: 25 V; and extraction time: 30 min). After extraction, the agarose gel was withdrawn and centrifuged for 5 min with 12000 rpm, to disrupt its framework to release the "trapped aqueous AP" apart from the gel structure. The separated AP was finally injected into the HPLC-UV for the analysis. The limits of detection (LODs) and recoveries in this proposed method were obtained 1.5 ng mL and 67.7 %-73.8 %, respectively. The system feasibility was examined by the quantification of model drugs in the real plasma and urine samples.
在本研究中，我们提出了一种新型的凝胶电膜萃取（G-EME）模式，即“内部”凝胶电膜萃取（IG-EME），用于从复杂生物样品中萃取吗啡和可待因作为模型碱性药物。在此，捕获在琼脂糖凝胶膜内部的水相介质同时充当凝胶膜和接受相（AP）。在这方面，该膜还充当分离过滤器（膜）和支撑液接受相（SLAP）。随着这一新技术的发展，G-EME过程中接受相体积的不必要变化（这是G-EME中由于电渗现象导致的常见问题）得到了妥善解决。简而言之，该装置包括将负极插入凝胶膜内部，正极插入供体相（DP）。随后，在最佳条件下（DP的pH值：6.0；膜组成（琼脂糖浓度：在pH值为3.0的水相介质中1%（w/v），厚度为15 mm）；电压：25 V；萃取时间：30分钟）轻松进行IG-EME。萃取后，取出琼脂糖凝胶并以12000 rpm离心5分钟，以破坏其框架，使“捕获的水相AP”从凝胶结构中释放出来。最终将分离出的AP注入高效液相色谱-紫外检测器进行分析。该方法的检测限（LOD）和回收率分别为1.5 ng/mL和67.7%-73.8%。通过对实际血浆和尿液样本中的模型药物进行定量，检验了该系统的可行性。
