Magdy Galal, Al-Enna Amira A, Belal Fathalla, El-Domany Ramadan A, Abdel-Megied Ahmed M
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Kafrelsheikh University, Kafrelsheikh, P.O. Box 33511, Egypt.
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura, P.O. Box 35516, Egypt.
R Soc Open Sci. 2022 Jun 1;9(6):220285. doi: 10.1098/rsos.220285. eCollection 2022 Jun.
In this study, highly fluorescent sulfur and nitrogen doped carbon quantum dots (S,N-CQDs) were used as fluorescent nanosensors for direct spectrofluorimetric estimation of each of gliclazide (GLZ) and saxagliptin (SXG) without any pre-derivatization steps for the first time. S,N-CQDs were synthesized employing a simple hydrothermal technique using citric acid and thiosemicarbazide. The produced S,N-CQDs were characterized using different techniques including fluorescence emission spectroscopy, UV spectrophotometry, high-resolution transmission electron microscopy and FT-IR spectroscopy. Following excitation at 360 nm, S,N-CQDs exhibited a strong emission peak at 430 nm. The native fluorescence of S,N-CQDs was quantitatively enhanced by addition of increased concentrations of the studied drugs. The fluorescence enhancement of S,N-CQDs and the concentrations of the studied drugs revealed a wide linear relationship in the range of 30.0-500.0 µM and 75.0-600.0 µM with limits of detection of 5.0 and 10.15 µM for GLZ and SXG, respectively. The proposed method was efficiently used for determination of cited drugs in their commercial tablets with % recoveries ranging from 98.6% to 101.2% and low % relative standard deviation values (less than 2%). The mechanism of interaction between S,N-CQDs and the two drugs was studied. Validation of the proposed method was carried out in accordance with International Conference on Harmonization (ICH) guidelines.
在本研究中,高荧光硫氮共掺杂碳量子点(S,N-CQDs)首次被用作荧光纳米传感器,用于直接荧光光谱法测定格列齐特(GLZ)和沙格列汀(SXG),无需任何预衍生步骤。采用柠檬酸和硫代氨基脲通过简单的水热技术合成了S,N-CQDs。使用包括荧光发射光谱、紫外分光光度法、高分辨率透射电子显微镜和傅里叶变换红外光谱在内的不同技术对制备的S,N-CQDs进行了表征。在360nm激发后,S,N-CQDs在430nm处呈现出强发射峰。通过添加浓度不断增加的研究药物,S,N-CQDs的固有荧光得到了定量增强。S,N-CQDs的荧光增强与研究药物的浓度在30.0 - 500.0µM和75.0 - 600.0µM范围内呈现出广泛的线性关系,GLZ和SXG的检测限分别为5.0和10.15µM。所提出的方法有效地用于测定市售片剂中的上述药物,回收率在98.6%至101.2%之间,相对标准偏差值较低(小于2%)。研究了S,N-CQDs与两种药物之间的相互作用机制。所提出方法的验证按照国际协调会议(ICH)指南进行。