El-Semary Mariam S, El-Emam Ali A, Belal F, El-Masry Amal A
Department of Medicinal Chemistry, Faculty of Pharmacy, Mansoura University 35516 Mansoura Egypt
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University 35516 Mansoura Egypt.
RSC Adv. 2023 Apr 6;13(16):11044-11054. doi: 10.1039/d3ra00824j. eCollection 2023 Apr 3.
A simple, rapid and eco-friendly method for synthesis of nitrogen and sulfur doped carbon dots (N,S-CDs) is described. The method involved one step carbonization assisted by a green microwave irradiation route using available and cheap sources, as sucrose (source for C) and thiourea (source for N and S). The formed aqueous solution of N,S-CDs showed excellent optical and electronic properties with high compatibility and stability. The particles of the prepared dots were spherical with a narrow range of size from 1.7 to 3.7 nm with a quantum yield of 0.20. These dots act as a fluorescent probe, as they showed an intense blue fluorescence at 413 nm after excitation at 330 nm. The N,S-CDs were utilized for determination of the anticoagulant drug, betrixaban maleate (BTM), based on quenching of their fluorescence upon its gradual addition. The quenching process was found to be through an inner filter effect mechanism. The proposed method showed a good linearity over a concentration range of (1.0-100.0 μM) with LOD and LOQ values of 0.33 μM and 0.99 μM, respectively. All validation parameters met the acceptance criteria according to ICH guidelines. The high specificity and sensitivity of the performed method contributed to further assay of BTM in dosage form and spiked human plasma sample with high percent recoveries and low values of RSD. Interference from co-administered drugs was studied. Finally, the greenness of the proposed method was evaluated adopting a ComplexGapi approach, the excellent green profile has supported its applicability in quality control laboratories.
本文描述了一种简单、快速且环保的合成氮硫共掺杂碳点(N,S-CDs)的方法。该方法采用绿色微波辐射路线辅助一步碳化,使用蔗糖(碳源)和硫脲(氮源和硫源)等易得且廉价的原料。所形成的N,S-CDs水溶液具有优异的光学和电学性质,具有高兼容性和稳定性。制备的碳点颗粒呈球形,粒径范围狭窄,为1.7至3.7 nm,量子产率为0.20。这些碳点可作为荧光探针,因为在330 nm激发后,它们在413 nm处发出强烈的蓝色荧光。基于逐渐加入马来酸贝曲西班(BTM)后荧光猝灭,N,S-CDs被用于测定抗凝血药物马来酸贝曲西班(BTM)。发现猝灭过程是通过内滤效应机制进行的。所提出的方法在(1.0 - 100.0 μM)浓度范围内显示出良好的线性,检测限(LOD)和定量限(LOQ)分别为0.33 μM和0.99 μM。根据国际人用药品注册技术协调会(ICH)指南,所有验证参数均符合验收标准。该方法的高特异性和灵敏度有助于进一步测定剂型和加标人血浆样品中的BTM,回收率高,相对标准偏差(RSD)值低。研究了同时给药药物的干扰情况。最后,采用ComplexGapi方法评估了所提出方法的绿色度,其优异的绿色特征支持了该方法在质量控制实验室中的适用性。