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Updated: Sep 12, 2025
High-throughput and Comprehensive Drug Surveillance Using Multisegment Injection-Capillary Electrophoresis-Mass Spectrometry
Published on: April 23, 2019
Investigation of illicit pregabalin in seized samples from Saudi Arabia
Fatimah M Alamri1,2, Sultan K Alshmmari3, Monerah A Altamimy3
1Department of Chemistry, College of Science, King Khalid University (KKU), Abha, Saudi Arabia.
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.
