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环保型 UV 分光光度法,采用磁性纳米复合聚合物提取和分析掺假食品中的性增强剂:计算机辅助设计的应用。

Eco-Friendly UV-Spectrophotometric Methods Employing Magnetic Nano-Composite Polymer for the Extraction and Analysis of Sexual Boosters in Adulterated Food Products: Application of Computer-Aided Design.

机构信息

Sohag University, Faculty of Pharmacy, Department of Pharmaceutical Analytical Chemistry, Sohag 82524, Egypt.

Egyptian Russian University, Faculty of Pharmacy, Department of Pharmaceutical Chemistry, Badr City, Cairo 11829, Egypt.

出版信息

J AOAC Int. 2023 Nov 2;106(6):1608-1619. doi: 10.1093/jaoacint/qsad084.

Abstract

BACKGROUND

Solid phase extraction (SPE) techniques, based on computationally designed magnetic-based multi-targeting molecular imprinted polymer (MT-MIP), combined with UV spectrophotometric approaches provide advantages in the examination of counterfeit samples.

OBJECTIVE

The current work describes an innovative and sustainable methodology for the simultaneous determination of tadalafil (TAD) and dapoxetine hydrochloride (DAP) in aphrodisiac counterfeit products (honey and instant coffee) utilizing SPE exploiting MT-MIP. Additionally, an innovative UV spectrophotometric method capable of resolving TAD in its pharmaceutical binary mixtures with DAP was developed. A novel computational approach was implemented to tailor the synthesis and design of the MT-MIP particles.

METHODS

We applied a newly developed UV spectrophotometric method which was based on a Fourier self-deconvolution (FSD) method coupled with the isoabsorptive point for determination of TAD and DAP in pharmaceutical dosage form. We also applied an SPE process based on MT-MIP designed particles, assisting in the analysis of both drugs in counterfeit food samples. The SPE process and the UV spectroscopic methodology were assessed regarding their greenness using the pioneering green analytical procedure index (GAPI), analytical greeness including sample preparation (AGREEprep) and AGREE tools. The synthesized MT-MIP particles were characterized by scanning electron microscopy and energy-dispersive x-ray spectroscopy.

RESULTS

The suggested spectrophotometric methods revealed a wide linear concentration range of 2-50 µg/mL with lower LODs in the range of 0.604-0.994 µg/mL. Additionally, the suggested method demonstrated the utmost sensitivity and eco-friendliness for their target in its mixed dosage form and counterfeit food products.

CONCLUSION

The SPE process and the developed analytical UV spectroscopic methodology were validated as per the ICH guidelines, and were found to be suitable for overseeing some counterfeiting activities in commercially available honey and instant coffee aphrodisiac products.

HIGHLIGHTS

An SPE method based on MT-MIP magnetic-based polymer and a UV spectroscopic method were successfully developed for analysis of TAD and DAP in different matrices.

摘要

背景

基于计算机设计的磁性多靶向分子印迹聚合物(MT-MIP)的固相萃取(SPE)技术,结合紫外分光光度法,在检查假冒样品方面具有优势。

目的

本研究描述了一种创新且可持续的方法,用于利用 SPE 技术从壮阳假药(蜂蜜和速溶咖啡)中同时测定他达拉非(TAD)和达泊西汀盐酸盐(DAP),该方法利用 MT-MIP 进行萃取。此外,还开发了一种能够分辨 TAD 与其与 DAP 制成的药物二元混合物的新型紫外分光光度法。采用一种新的计算方法来调整 MT-MIP 颗粒的合成和设计。

方法

我们应用了一种新开发的紫外分光光度法,该方法基于傅里叶自解卷积(FSD)法,并结合等吸收点,用于测定药物制剂中的 TAD 和 DAP。我们还应用了基于 MT-MIP 设计颗粒的 SPE 工艺,以辅助分析假药中的两种药物。采用开创性的绿色分析程序指数(GAPI)、包括样品制备(AGREEprep)和 AGREE 工具的分析绿色度(AGREE),评估 SPE 过程和紫外光谱方法的绿色度。合成的 MT-MIP 颗粒通过扫描电子显微镜和能量色散 X 射线光谱进行表征。

结果

所提出的分光光度法显示出 2-50μg/mL 的宽线性浓度范围,LOD 值在 0.604-0.994μg/mL 范围内较低。此外,在所研究的混合制剂和假药产品中,所提出的方法在其混合制剂和假药产品中表现出对其目标物的最高灵敏度和生态友好性。

结论

根据 ICH 指南对 SPE 过程和开发的分析紫外光谱方法进行了验证,发现它们适用于监测市售蜂蜜和速溶咖啡壮阳产品中的一些假冒活动。

重点

成功开发了基于 MT-MIP 磁性聚合物的 SPE 方法和紫外分光光度法,用于不同基质中 TAD 和 DAP 的分析。

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