Zeraatkar Moghaddam Ali, Goharjoo Maryam, Ghiamati Ebrahim, Khodaei Kamal, Tabani Hadi
Department of Chemistry, Faculty of Science, University of Birjand, Birjand, South Khorasan, Iran.
Department of Chemistry, Faculty of Science, University of Birjand, Birjand, South Khorasan, Iran.
Talanta. 2021 Jan 15;222:121557. doi: 10.1016/j.talanta.2020.121557. Epub 2020 Aug 24.
In this work, gel electro-membrane extraction (G-EME) method is suggested for extraction and determination of propranolol and atenolol in complex biological samples. An in-house membrane based on agarose was used as green and biodegradable gel membrane. Essential chemical parameters that influence on extraction efficiency were tested, optimized and evaluated via a central composite design (CCD) and response surface methodology (RSM). Optimal conditions for extraction of drugs from the 7.0 mL sample were as follows: 3% (w/v) agarose with 0.1% (v/v) acetic acid functioning as membrane, voltage: 50 V; pH of the donor phase (DP): 8.1; pH of the AP: 3.3; extraction time: 35.9 min. Under these conditions, the acceptable normalized extraction recoveries were obtained such as 71.9 ± 5.4% that were in good agreement with the predicted values (i.e., 73.1 ± 0.9%). Limits of detection (LODs) for propranolol and atenolol were 5.0 ng mL and 7.5 ng mL, respectively. Moreover, for the first time, the effect of presence of four graphene-based nanomaterials such as graphene (G), graphene oxide (GO), three-dimensional nitrogen doped graphene oxide (3D-ND-GO) and high nitrogen doped graphene oxide (HND-GO) in agarose gel membrane on extraction efficiency, was investigated. The results showed that in presence of these nanomaterials, the normalized recovery depressed significantly due to increasing of electric current and electroendosmosis (EEO) phenomenon. Eventually, the proposed method was applied to quantify basic drugs in real plasma samples with relative recoveries in the range of 85.7-97.5%, indicating good reliability of the assay.
在本研究中，提出了凝胶电膜萃取（G-EME）法用于复杂生物样品中普萘洛尔和阿替洛尔的萃取与测定。使用基于琼脂糖的自制膜作为绿色可生物降解的凝胶膜。通过中心复合设计（CCD）和响应面方法（RSM）对影响萃取效率的关键化学参数进行了测试、优化和评估。从7.0 mL样品中萃取药物的最佳条件如下：3%（w/v）琼脂糖与0.1%（v/v）乙酸作为膜，电压：50 V；供体相（DP）pH值：8.1；接受相（AP）pH值：3.3；萃取时间：35.9分钟。在这些条件下，获得了可接受的归一化萃取回收率，如71.9±5.4%，与预测值（即73.1±0.9%）高度吻合。普萘洛尔和阿替洛尔的检测限（LOD）分别为5.0 ng/mL和7.5 ng/mL。此外，首次研究了琼脂糖凝胶膜中四种基于石墨烯的纳米材料，即石墨烯（G）、氧化石墨烯（GO）、三维氮掺杂氧化石墨烯（3D-ND-GO）和高氮掺杂氧化石墨烯（HND-GO）的存在对萃取效率的影响。结果表明，在这些纳米材料存在的情况下，由于电流增加和电渗现象（EEO），归一化回收率显著降低。最终，所提出的方法应用于实际血浆样品中碱性药物的定量分析，相对回收率在85.7-97.5%范围内，表明该分析方法具有良好的可靠性。
