Karolina Pioruńska-Sędłak

This study presents the results of a multi-technique forensic investigation of suspicious soft capsules seized by law enforcement during a criminal case. The unlabeled samples, sold as therapeutic and “regenerative” food supplements, were examined using liquid chromatography–tandem mass spectrometry (LC-MS/MS), Fourier-transform infrared spectroscopy with attenuated total reflection (ATR-FTIR), chemiluminescence, and brightfield/confocal microscopy. These complementary analytical approaches revealed that the capsules contained biological material of unknown origin, including blood-derived compounds, lipid constituents, and cellular structures. The findings indicate biological adulteration, possibly due to deliberate falsification or severe contamination. To place these results in a broader biomedical context, a scoping review of literature on blood- and tissue-derived materials used in biomedical and nutraceutical applications was conducted. This review underscores how such products are developed, promoted, and regulated, highlighting the potential health and biosafety risks associated with unregulated biologically themed supplements. Overall, this study demonstrates a transferable analytical workflow suitable for forensic laboratories and emphasizes the need for continued regulatory vigilance to protect public health. Given the evidentiary constraints typical of forensic casework—specifically, the small amount of seized material—the workflow was optimized to maximize information yield through minimally destructive, orthogonal, non-genetic screening methods, with LC-MS/MS reserved for final molecular confirmation. DNA typing was not performed because, after confirmatory analyses, the remaining material was insufficient for reliable genotyping.

This study presents a methodology for developing a cyclodextrin-based delivery system for ceftobiprole, a poorly water-soluble and amphoteric drug, chemically stable in acidic conditions. Ceftobiprole is a broad-spectrum cephalosporin antibiotic administered clinically as its water-soluble prodrug, ceftobiprole medocaril, due to limited aqueous solubility of the parent compound. Solubility enhancement was achieved through complexation with anionic sulfobutylether-β-cyclodextrin (SBE-β-CD). At a pH below 3, ceftobiprole is protonated and cationic, which facilitates electrostatic interactions with the anionic cyclodextrin. An optimised high-performance liquid chromatography (HPLC) method was used to assess solubility, the impurity profile, and long-term chemical stability. X-ray powder diffraction (XRPD) confirmed the amorphous nature of the system and the absence of recrystallization. Nuclear magnetic resonance (NMR) and attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy supported the formation of a host–guest complex. The freeze-dried system prepared from 0.1 M formic acid solution contained negligible residual acid due to nearly complete sublimation. The most promising formulation was a ternary system of ceftobiprole, maleic acid, and SBE-β-CD (1:25:4 molar ratio), showing ~300-fold solubility improvement, low levels of degradation products, and stability after eight months at −20 °C. After pH adjustment to a parenterally acceptable level, the formulation demonstrated solubility and a pH comparable to the marketed drug product.

Have you ever looked at a powder diffractogram during a routine qualitative test and wondered how much of a particular powder compound is in the powder material? Several methods can work this out, but none of them could be used in our case because something was missing from each in performing a rapid quantity test for an active ingredient in a tablet. A semiquantitative method of an X-ray powder diffraction analysis of products containing sildenafil citrate is proposed. This method utilizes calibration curves for the most common compositions encountered in falsified and not-registered Viagra analogues. Sildenafil doses are established for singularly prepared powder probes of a medicinal product, and two runs of data collection are used: the first, the fast one, for the qualitative analysis of the product, and the second for selected 2θ regions for the API and identified excipients. An example of a product composed mainly of sildenafil citrate, gypsum and microcrystalline cellulose is discussed in detail. The data obtained from X-ray experiments were compared with the results obtained from validated liquid chromatography coupled to a diode array detector and mass spectrometry methods.