对沙特阿拉伯查获样本中非法普瑞巴林的调查。

Investigation of illicit pregabalin in seized samples from Saudi Arabia.

作者信息

Alamri Fatimah M, Alshmmari Sultan K, Altamimy Monerah A, Al Othaim Ibrahim A, Alshehri Yahya M, Alafraa Rayed M, Almalki Ahmed D, Alkhalifah Turki A, Sahlabji Taher, Idris Abubakr M, Al-Hamoud Haitham, Jamous Yahya F, Aldawasri Fahad S

机构信息

Department of Chemistry, College of Science, King Khalid University (KKU), Abha, Saudi Arabia.

Department of Chemistry, College of Science, University of Bisha (UB), Bisha, Saudi Arabia.

出版信息

Front Chem. 2025 Jul 23;13:1594567. doi: 10.3389/fchem.2025.1594567. eCollection 2025.

DOI:10.3389/fchem.2025.1594567

PMID:40771717

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC12326260/

Abstract

INTRODUCTION

Pregabalin (PGL) is a medication that is prescribed for controlling specific neurological-related symptoms. Due to its abuse in multiple countries, PGL has been classified as a controlled substance by authorities, including the Saudi Food and Drug Authority (SFDA).

METHODS

This study developed a validated ultra-performance liquid chromatography-photodiode array detector (UPLC-PDA) method to quantify PGL in 40 seized samples (35 capsules, 5 powders). A complementary liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was used to detect potential adulterants.

RESULTS

The UPLC-PDA method demonstrated linearity (r = 0.9973) for PGL quantification (0.50-3.00 mg/mL), with an accuracy of 96%-102%. The RSD% values were 0.63% and 1.03% for intra-day and inter-day precision, respectively. Analysis of the five powder samples revealed a relative inconsistency in PGL content (107.91%-114.55%). Moreover, it showed higher variability in PGL content (RSD 1.16%-5.30%), suggesting possible adulteration or poor manufacturing. Furthermore, the results of the nuclear magnetic resonance (NMR) showed an acceptable purity for the powder samples. On the other hand, among 35 capsules, 5 (14.29%) exceeded pharmacopeial limits (95%-105% PGL content), while 6 (17.14%) contained <95% PGL.

DISCUSSION

These results demonstrate significant variability in PGL content and the presence of adulterants, underscoring the need for robust analytical methods in forensic chemistry. Furthermore, the LC-MS/MS method detected adulteration of PGL with codeine, paracetamol, and gabapentin in 2.9% of the analyzed capsules, suggesting custom mixing by perpetrators. In general, 31.43% of these samples failed to meet quality standards and contained substances beyond declared contents that posed toxicity risks, revealing inadequacies in illicit drug production and circulation. The UPLC-PDA method offers a rapid, validated approach for PGL quantification, while LC-MS/MS enhances adulterant detection, supporting forensic and quality control applications.

摘要

引言

普瑞巴林（PGL）是一种用于控制特定神经相关症状的药物。由于其在多个国家被滥用，PGL已被包括沙特食品药品管理局（SFDA）在内的当局列为管制物质。

方法

本研究开发了一种经过验证的超高效液相色谱 - 光电二极管阵列检测器（UPLC - PDA）方法，用于对40份查获样品（35粒胶囊、5份粉末）中的PGL进行定量。采用互补的液相色谱 - 串联质谱（LC - MS/MS）方法检测潜在的掺假物质。

结果

UPLC - PDA方法在PGL定量（0.50 - 3.00 mg/mL）方面表现出线性（r = 0.9973），准确度为96% - 102%。日内和日间精密度的相对标准偏差（RSD%）值分别为0.63%和1.03%。对5份粉末样品的分析显示，PGL含量存在相对不一致性（107.91% - 114.55%）。此外，其PGL含量的变异性较高（RSD为1.16% - 5.30%），表明可能存在掺假或生产工艺不佳的情况。此外，核磁共振（NMR）结果显示粉末样品的纯度可接受。另一方面，在35粒胶囊中，有5粒（14.29%）超过了药典规定的限度（PGL含量为95% - 105%），而有6粒（17.14%）的PGL含量低于95%。

讨论

这些结果表明PGL含量存在显著变异性且存在掺假物质，凸显了法医化学中采用可靠分析方法的必要性。此外，LC - MS/MS方法在2.9%的分析胶囊中检测到PGL与可待因、对乙酰氨基酚和加巴喷丁掺假，表明作案者进行了定制混合。总体而言，这些样品中有31.43%不符合质量标准，含有超过申报含量且具有毒性风险的物质，揭示了非法药物生产和流通中的不足之处。UPLC - PDA方法为PGL定量提供了一种快速、经过验证的方法，而LC - MS/MS增强了掺假物质的检测，支持法医和质量控制应用。