Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Mansoura University, P.O. Box 35516, Mansoura, Egypt.
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Kafrelsheikh University, P.O. Box 33511, Kafrelsheikh, Egypt.
Sci Rep. 2022 Jun 7;12(1):9372. doi: 10.1038/s41598-022-13194-1.
In this study, sensitive, facile, and cost-effective spectrofluorimetric approaches were developed for the determination of pholcodine and ephedrine. Method I is a novel spectrofluorimetric method depending on measuring the native fluorescence of pholcodine at 337 nm after excitation at 284 nm over a concentration range of 0.01-2.4 μg/mL. The method sensitivity reached quantitation and detection limits down to 10.0 and 5.0 ng/mL, respectively. Method II relied on the simultaneous estimation of pholcodine and ephedrine using synchronous fluorimetry for the first time. The cited drugs were measured concurrently at 286 and 304 nm for pholcodine and ephedrine, respectively at Δλ of 40 nm without interference. Excellent linear relationship between concentration and response was obtained over the ranges of 0.05-6.0 μg/mL and 0.02-1.0 μg/mL for pholcodine and ephedrine, respectively. The method showed distinct sensitivity and exhibited quantitation limits of 20.0 and 10.0 ng/mL and detection limits of 10.0 and 5.0 ng/mL, respectively. The method was successfully applied to the syrup dosage form. The two developed approaches were also applied to in-vitro plasma samples, showing good bioanalytical applicability and providing further insights for monitoring drug abuse. The proposed methods were validated according to ICHQ2(R1) guidelines. The proposed methodologies' greenness profiles were evaluated using two greenness assessment tools.
在这项研究中，开发了灵敏、简便、经济高效的分光荧光法来测定可待因和麻黄碱。方法 I 是一种新颖的分光荧光法，依赖于在 284nm 激发下测量 0.01-2.4μg/mL 浓度范围内可待因的固有荧光，在 337nm 处测量。该方法的灵敏度达到了定量和检测限，分别为 10.0 和 5.0ng/mL。方法 II 首次依赖同步荧光法同时估计可待因和麻黄碱。在没有干扰的情况下，分别在 286nm 和 304nm 处测量可待因和麻黄碱的 Δλ 为 40nm。可待因和麻黄碱的浓度与响应之间均获得了优异的线性关系，范围分别为 0.05-6.0μg/mL 和 0.02-1.0μg/mL。该方法具有明显的灵敏度，定量限分别为 20.0 和 10.0ng/mL，检测限分别为 10.0 和 5.0ng/mL。该方法已成功应用于糖浆剂型。所开发的两种方法也已应用于体外血浆样品，显示出良好的生物分析适用性，并为监测药物滥用提供了进一步的见解。根据 ICHQ2(R1)指南验证了所提出的方法。使用两种绿色评估工具评估了所提出方法的绿色度概况。
