This study proposed a new method of EME based on agarose gel named rotating electrode gel electromembrane extraction (RE-G-EME) for extraction and determination of naloxone, naltrexone, and nalbuphine as basic drugs from real human urine samples. In this new method, a rotating electrode connected to the armature was used to agitate the acceptor phase (AP). With this new development, the extraction efficiency enhanced due to increasing analytes mass transfer from gel membrane interface toward the AP. The effective parameters on the extraction efficiency were optimized and the maximum recoveries of the analytes were obtained under the optimal extraction conditions (3.0% (w/v) agarose with pH 5.0 as gel membrane; voltage: 25 V; pH of the donor phase (DP): 6.0; pH of the AP: 4.0; stirring rate of the DP: 750 rpm; electrode rotation speed within AP: 125 rpm; extraction time: 25 min). The method offered limits of detection (LODs) and extraction recoveries in the range of 0.3–1.5 ng mL⁻¹, and 74.3% − 87.0%, respectively. Also, the repeatability of the proposed method was measured for four repeated experiments and was in the acceptable range of 4.3% − 8.1%. To understand the influence of agitation of the AP on the extraction efficiency, a comparative study was carried out between conventional G-EME and RE-G-EME methods. The results showed that, for short the extraction times (t ≤ 10 min), extraction efficiency of G-EME was almost the same as that of RE-G-EME. However, at longer extraction times (25 min), the extraction efficiency of RE-G-EME was significantly higher than that of G-EME. Finally, the proposed method was successfully applied to determine concentrations of model drugs in real urine samples with relative recoveries of 81.1–96.1% indicating good reliability of the proposed method.

这项研究提出了一种新的基于琼脂糖凝胶的EME方法，称为旋转电极凝胶电膜提取（RE-G-EME），用于从真实的人类尿液样品中提取和测定纳洛酮，纳曲酮和纳布啡作为基本药物。在这种新方法中，使用连接到电枢的旋转电极来搅动受体相（AP）。随着这一新的发展，由于分析物从凝胶膜界面向AP的质量转移增加，萃取效率得到了提高。优化了萃取效率的有效参数，并在最佳萃取条件下（3.0％（w / v）琼脂糖，pH 5.0作为凝胶膜；电压：25 V；供体相的pH（ DP）：6.0； AP的pH：4.0； DP的搅拌速度：750 rpm； AP内的电极转速：125 rpm; 提取时间：25分钟）。该方法提供的检出限（LOD）和提取回收率在0.3–1.5 ng mL范围内^-1和74.3％-87.0％。此外，针对四个重复的实验测量了所提出方法的重复性，其可接受范围为4.3％-8.1％。为了了解AP的搅拌对提取效率的影响，在常规G-EME和RE-G-EME方法之间进行了比较研究。结果表明，在较短的萃取时间（t≤10分钟）内，G-EME的萃取效率几乎与RE-G-EME相同。但是，在更长的提取时间（25分钟）下，RE-G-EME的提取效率显着高于G-EME。最终，该方法成功应用于实际尿液样品中模型药物的浓度测定，相对回收率为81.1–96.1％，表明该方法具有良好的可靠性。