Nano-scale multi-spectroscopic analysis of the anti-fibromyalgia drug pregabalin based on dihydropyridine ring formation with sustainability and whiteness evaluation.

Mohamed A El Hamd, Reem H Obaydo, Marwa Ibrahim Helmy, Wael A Mahdi, Sultan Alshehri, Mahmoud El-Maghrabey, Christine K Nessim
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Abstract

This research addresses the challenge of analyzing pregabalin, a primary amine in a zwitterionic structure, which is difficult to evaluate due to its lack of chromatophore. The study introduces a derivatization assessment using Hantzsch's multicomponent organic reaction to enhance the detectability of pregabalin by forming a highly fluorescent dihydropyridine derivative. This process involves the condensation of pregabalin with acetylacetone and formaldehyde, yielding a yellowish-green compound measurable both colorimetrically at 338 nm and fluorimetrically at an emission wavelength of 486 nm (λexcitation = 408 nm). The reaction conditions were thoroughly optimized to obtain the highest possible sensitivity, reduce reagent and time consumption, and use safe solvents. The developed method displayed high sensitivity and linearity in the concentration ranges of 4.0 - 20.0 µg/mL in colorimetric assay and reached a nano-scale analysis level of 40 - 2000 ng/mL with a detection limit down to 10 ng/mL when adopting the fluorimetric measurement. Both assessments were rigorously evaluated for their performance, adhering to the International Conference on Harmonization (ICH) standards. The accuracy of these methods was confirmed through the recovery rates of real samples, showing 98.9 ± 0.2 % for colorimetric and 98.2 ± 0.7 % for fluorimetric assessment. The excellent sensitivity of the suggested spectrofluorometric approach led to its use in the measurement of PRG in spiked human urine samples, resulting in particularly good recoveries ranging from 95.3 to 102.8 %. Meanwhile, the Need, Quality, Sustainability (NQS) index looks into how necessary the method is, execution quality (evaluated using the RGB 12 algorithm), and how it fits with the Sustainable Development Goals (SDGs), underlining the benefits of employing natural reagents. The developed approach showed superiority in sensitivity and sustainability compared to previous analytical approaches for pregabalin.

基于二氢吡啶环形成的抗纤维肌痛药物普瑞巴林的纳米级多光谱分析以及可持续性和白度评估。
普瑞巴林是一种具有齐聚物结构的伯胺,由于缺乏色素,很难对其进行评估,本研究正是要解决这一难题。该研究介绍了一种衍生化评估方法,利用汉茨氏多组分有机反应,通过形成一种高荧光二氢吡啶衍生物来提高普瑞巴林的可检测性。这一过程涉及普瑞巴林与乙酰丙酮和甲醛的缩合,生成的黄绿色化合物可在 338 纳米波长下进行比色测量,在 486 纳米波长下进行荧光测量(λ 激发 = 408 纳米波长)。为了获得尽可能高的灵敏度、减少试剂和时间消耗以及使用安全溶剂,对反应条件进行了全面优化。所开发的方法在比色法检测的 4.0 - 20.0 µg/mL 浓度范围内显示出较高的灵敏度和线性度;在采用荧光法检测时,可达到 40 - 2000 ng/mL 的纳米级分析水平,检测限低至 10 ng/mL。这两项评估均按照国际协调会议(ICH)标准对其性能进行了严格评估。真实样品的回收率证实了这些方法的准确性,比色法的回收率为 98.9 ± 0.2 %,荧光法的回收率为 98.2 ± 0.7 %。建议采用的光谱荧光测定法灵敏度极高,因此可用于测量加标人体尿样中的 PRG,回收率特别高,达到 95.3% 至 102.8%。同时,需求、质量、可持续性(NQS)指数考察了该方法的必要性、执行质量(使用 RGB 12 算法评估)以及与可持续发展目标(SDGs)的契合程度,强调了使用天然试剂的益处。与以前的普瑞巴林分析方法相比,所开发的方法在灵敏度和可持续性方面更具优势。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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