Search Results (37)

Probiotics are live microorganisms that provide health benefits when administered in adequate amounts. Due to the increasing popularity of probiotic supplements, concerns have arisen regarding their quality, microbial composition, and safety. This study aimed to evaluate the quantitative and qualitative characteristics of the selected probiotics available on the Polish market, including both dietary supplements and foods for special medical purposes, and to compare the obtained results with the information provided on the product labels. Fifteen commercial probiotic products were analysed. Viable microorganism counts were determined using the traditional culture-based plate count method and by flow cytometry for selected products. Species identification was performed using MALDI-TOF MS and qPCR, whereas microbiological purity testing was conducted to confirm the absence of pathogenic bacteria. Significant differences were observed between the declared and experimentally determined numbers of viable microorganisms. Only a few products maintained bacterial counts consistent with label claims, while most contained considerably low viable cells. Flow cytometry revealed higher viable cell counts than plate counting, indicating the presence of viable but non-culturable bacteria. The declared species composition of the strains was mostly confirmed, although in several cases, undeclared probiotic microorganisms were identified. All tested products were free from pathogens. The study indicates significant discrepancies in the quality of probiotic supplements available on the Polish market. From a consumer perspective, these findings highlight the importance of verifying probiotic quality and suggest that not all commercial products may guarantee the full range of claimed health benefits. The implementation of standardised analytical procedures and enhanced quality control measures is therefore essential to ensure the product safety, strain authenticity, and reliability of health-related claims. Full article

Background/Objectives: Laser has a prominent place in pharmaceutical industry, especially in the marking of solid dosage forms (SDFs). To combat falsified medicines, this study evaluates QR code marking on the surface of tablets as a supplement to serialization on packaging, using an ultrafast laser to achieve industrially relevant marking speeds while preserving the functional integrity of double film-coated ibuprofen tablets. Methods: Tablets were directly compressed and coated with a double film: the inner layer was a gastro-resistant coating (Acryl-EZE^® MP), while the outer one was a coloured, TiO₂-containing (TC) or TiO₂-free (TF) immediate-release coating (Opadry^®). QR codes were ablated on the tablet surface using various laser parameters (e.g., pulse energy and scanning speed), and the effects were physically, chemically, and microscopically examined to evaluate their properties after this processing. Results: No significant differences were observed between TC and TF coatings. In addition, the readability of QR code is strongly influenced by laser settings and coating types. Furthermore, the used laser has achieved the expected fast marking speed and high-precision coding, which may be economically feasible for pharmaceutical companies. According to the profilometry findings, the ablation depth could be compensated for with an appropriate coating thickness to enable the desired release properties. This was confirmed by the results of SEM, Raman analysis, and in vitro dissolution test. Conclusions: Ultrafast Ti:Sa laser-based QR code marking directly onto the dosage form offers increasing benefits in the healthcare field. However, it may undesirably affect the behavior of the dosage form. This requires careful consideration of formulation and laser processing conditions before application, especially in the case of delayed-release (DR) systems. Full article

Background/Objectives: This study aimed to perform a comparative analysis of the original Viagra^® product and sildenafil-containing tablets obtained from illegal sources (the darknet). Specifically, the analyzed material consisted of samples seized by Polish law enforcement authorities from unverified vendors operating within the Central European darknet market. The study utilized thermal methods, specifically Thermogravimetry (TG), Derivative Thermogravimetry (DTG), and calculated Differential Thermal Analysis (c-DTA), as well as colorimetric analysis based on the International Commission on Illumination (CIE) L*a*b* system. Methods: Thermal analyses enabled the assessment of the thermal stability of the tested samples, identification of characteristic stages of thermal decomposition, and determination of differences in thermal behavior between the pure substance, the original preparation, and darknet samples. In turn, color measurements in the CIE L*a*b* space allowed for an objective comparison of tablet appearance and determination of the degree of color similarity to the original product. Results: The obtained results showed that only a few samples (V1, V3, V4, V6, V8) exhibited features similar to the original Viagra^®, both in terms of thermal profile and color. Most of the tested tablets were characterized by significant variability in physicochemical properties, indicating a lack of quality control and inconsistency in formulation. Samples V2 and V7 deviated particularly strongly—both thermally and visually—suggesting that they might not contain the original active substance or contained it in a different chemical form. Conclusions: The use of combined thermal and colorimetric methods proved to be an effective tool in the identification of counterfeit pharmaceutical products, enabling simultaneous evaluation of their composition and authenticity. The results confirm the validity of employing integrated physicochemical analyses for the detection of falsified medicines present on the illegal market. Full article

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. Full article

This study aimed to assess the extent of vitamin B₁ and B₆ vitamer loss during a single peritoneal dialysis (PD) session using a combination of chromatographic techniques and chemometric analysis. Dialysis effluent samples were collected from 41 PD patients (22 on continuous ambulatory peritoneal dialysis (CAPD) and 19 on automated peritoneal dialysis (APD)) during a standardised peritoneal equilibration test. Concentrations of thiamine monophosphate, thiamine diphosphate (ThDP), pyridoxine, pyridoxal (PL), and pyridoxamine were determined using high-performance liquid chromatography with a fluorescence detector. The analytical method was validated in terms of sensitivity, linearity, accuracy, and recovery. Multiple regression analysis was employed to identify potential clinical and demographic predictors of vitamin washout. All vitamers except pyridoxal 5-phosphate (PLP) were detectable in dialysis effluents. ThDP exhibited the greatest loss among the B₁ forms (ca. 0.05–0.57 mg/24 h), while PL exhibited the most significant loss among the B₆ forms (ca. 0.01–0.19 mg/24 h). Vitamin losses varied depending on the dialysis modality (continuous ambulatory peritoneal dialysis, or CAPD, versus automated peritoneal dialysis, or APD) and the peritoneal transport category. Regression analysis identified body weight, haemoglobin, and haematocrit as independent predictors of ThDP washout (R² = 0.58). No statistically robust models were established for the other vitamers. Even short medical procedures (such as single PD) can result in measurable losses of water-soluble vitamins, particularly ThDP and PL. The results emphasise the importance of personalised vitamin supplementation for PD patients and suggest that body composition and haematological parameters significantly influence the loss of thiamine. Full article

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. Full article

The World Health Organization (WHO) Global Benchmarking Tool (GBT) classifies regulatory systems into four maturity levels, with Maturity Level 3 (ML3) signifying a stable and effective regulatory environment. As of January 2025, eight African nations—Egypt, Ghana, Nigeria, Rwanda, Senegal, South Africa, Tanzania, and Zimbabwe—have attained ML3 status, marking a significant milestone in the continent’s regulatory landscape. Achieving ML3 confers critical benefits, including reducing substandard and falsified medicines, which enhances public health safety and fosters trust in healthcare systems. This progress encourages local manufacturing, diminishing reliance on imported medicines and promoting economic development. Furthermore, ML3 NRAs are better equipped to address public health emergencies, enabling swift approvals for vaccines and therapeutics while upholding safety standards. Nonetheless, challenges persist, including fragmented regulatory systems, the prevalence of counterfeit medicines, and limited resources. Overcoming these hurdles necessitates enhanced organizational capacity, investments in training, and the promotion of collaboration among NRAs. There is an urgent call for greater political commitment and resource allocation to strengthen regulatory systems across Africa. Achieving and maintaining ML3 status is essential for enhancing medicine regulation, supporting local manufacturing, and improving public health outcomes across the continent. While progress has been made, sustained efforts are crucial to tackling existing challenges and harnessing the full potential of advanced regulatory frameworks. Full article

In recent years, an increasing number of case reports have mentioned the presence of illicit nootropics, smart drugs or mind doping products on the market. To better understand the extent of the problem, a market surveillance study was organised by the General European Official Medicines Control Laboratory Network and associated member Australia to detect substandard, falsified or illegal medicines or dietary supplements containing unauthorised nootropic molecules of natural or synthetic origin. From January 2020 to September 2024, 159 different samples were documented, which yielded a comprehensive dataset of 166 molecular identification entries. Within this dataset, 34 distinct molecules were identified. Most samples were sold or presented as dietary supplements (49%) or medicines (32%). The vast majority (69%) were collected from the illegal market. Prescription drugs and non-authorised drugs only available on prescription in Russia were found in pharmacological quantities; some of the latter (noopept, phenylpiracetam and phenibut) were intercepted as large bulk quantities of raw material. Unauthorised novel foods, prescription or higher amounts of melatonin, and clinically uncharacterised research molecules were also reported. This study highlights the need for more active monitoring and screening of such products, as consumption of some of the reported samples could have detrimental health effects. Furthermore, as a large number of the samples were presented as dietary supplements, consumers may not be aware of the possible dangers and side-effects of these products. Full article

The presence of substandard and falsified (SF) medicines poses a significant challenge in resource-limited countries. Low-quality antibiotics are commonly reported in low-income countries. The present study aimed to develop and validate a liquid chromatography method with ultraviolet detection (LC-UV) for the identity screening and assay of 13 different injectable antibiotics, i.e., cefepime, amoxicillin, cefazolin, ampicillin, chloramphenicol, ceftazidime, ceftriaxone, cefotaxime, vancomycin, flucloxacillin, cloxacillin, benzylpenicillin, and meropenem in pharmaceutical formulations. Separation was performed using an XBridge C18 column and gradient elution. Mixtures of acetonitrile and 20 mM phosphate buffer (pH 8.0) were used as the mobile phases. The screening method was validated in terms of specificity and robustness, while linearity, precision, accuracy, and sensitivity were checked for the quantification method. The determination coefficients (R²) following linear regression were all greater than 0.999. The method showed good precision, with relative standard deviation values below 1%. The percentage recovery values were close to 100%. The method was applied to analyze 17 injectable antibiotics collected from the Ethiopian market. All commercial samples analyzed contained the correct API and met USP content specifications. Full article

Plant-based food supplements (FS) of doubtful traceability have now emerged as a new threat to human health. Food supplements adulterated with pharmaceutical ingredients are considered “medicines in disguise” by regulatory authorities, which is a sub-category of falsified medicines. In the context of illegal manufacture and trade, as well as in the absence of an official phyto- and/or pharmacovigilance system, emergency departments and poison control centers constitute a early warning system for detecting ingested suspect FS. In the present investigation, we set up efficient workflows for the systematic characterization of adulterated plant-based FS in the context of an original local early warning alert system (i.e., FalsiMedTrack) involving an emergency department, a poison center, and academic analytical chemistry laboratories. Fit-for-purpose cross-analytical methods were employed, including sophisticated methods such as liquid chromatography coupled to high-resolution mass spectrometry, nuclear magnetic resonance, X-ray powder diffraction, as well as the most accessible and affordable HPLC method with UV/DAD detection. The strategy was applied successfully to typical cases of suspect plant-based health products, i.e., sample incriminated in patients experiencing side effects and herbal products currently commercialized for their “amazing health benefits”. The samples contained active pharmaceutical ingredients, including diclofenac, piroxicam, dexamethasone 21-acetate, and sibutramine. We provided evidence of “medicines in disguise” presented as food supplements, which raises concerns about their quality and safety. Full article

The evolution of medical reasoning is deeply intertwined with philosophical thought, beginning with Aristotle’s foundational work in deductive logic. Aristotle’s principles significantly influenced early medical practice, shaping the works of Galen and Avicenna, who made empirical observations that expanded clinical knowledge. During the Enlightenment, both inductive reasoning, as advocated by Francis Bacon, and deductive methods, as stressed by René Descartes, significantly advanced medical reasoning. These approaches proved insufficient when it came to handling uncertainty and variability in medical outcomes. Nineteenth-century figures like William Osler advanced a probabilistic understanding of medicine. Karl Popper’s 20th-century hypothetico-deductive method, which introduced the concept of falsifiability and transformed scientific inquiry into a rigorous process of hypothesis testing, is a fundamental aspect of evidence-based medicine (EBM). EBM emerged as the dominant paradigm, combining empirical research, clinical expertise, and statistical inference to guide medical decisions. Looking forward, Bayesian reasoning offers a further refinement in medical reasoning. By incorporating prior knowledge and continuously updating probabilities with new evidence, Bayesianism addresses the limitations of frequentist methods and offers a more dynamic and adaptable framework for clinical decision making. As medical reasoning evolves, understanding this philosophical lineage is essential to navigating the future of patient care, where evidence must be both rigorously tested and individually tailored. Full article

The GPHF-Minilab™ is a portable toolkit for performing qualitative methods such as thin-layer chromatography (TLC) on common pharmaceuticals. It is particularly useful in resource-limited locations where it is more challenging to monitor for substandard and falsified (SF) medicines. However, the GPHF-Minilab™ TLC methods are only semi-quantitative at best and thus have issues monitoring product quality effectively. We have improved on the GPHF-Minilab™ TLC method for metronidazole, a common antibiotic, by making it fully quantitative. Sample solutions were spotted on TLC plates alongside three metronidazole standards at different concentrations. After development, plates were imaged in a lightbox with two different smartphone cameras. Images were processed through the open-source program ImageJ and resulting pixel data from the standard spots were used to create a calibration curve, enabling quantitation of the sample. The USP Metronidazole Tablet high-performance liquid chromatography (HPLC) assay was used as the reference method. We validated this TLC method using 250 and 500 mg metronidazole tablets from different manufacturers and assessed linearity, range, accuracy, precision, intermediate precision, specificity, and robustness. These improvements should enhance the GPHF-Minilab™ TLC methods for metronidazole product screening. Additionally, the procedure is extensible to other analytes, although further validation would be required for each Minilab method. Full article

A hand-held NIR spectrophotometric method was developed, validated, and applied for the determination of tadalafil in tablets. The aim of our work was to develop analytical methods based on vibrational techniques using low-cost portable equipment. Based on different chemometric modeling, we attempted to validate the method, which gave encouraging results from the principal component analysis (PCA), DD-SIMCA, and PLS modeling. Following this, we optimized the method using an appropriate experiment plan. For validation, we used the total error approach with acceptance limits set at ±10% with a risk level of 5%. The method showed that it was possible to perform both qualitative and quantitative analysis of pharmaceutical products using low-cost portable NIR systems with chemometric tools. The developed approach enabled the completion of the first step in implementing an NIR method for quality control of tadalafil-based drugs in the DRC. Validation difficulties of the PLS method resulted from the lack of information about inter-day serial variations of spectral responses. It would be interesting to extend the study to a larger calibration interval in order to correct uncertainties that may result from the variability observed under different conditions and to verify robustness. These are the limitations of this work, but the results are nevertheless very encouraging. Full article

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. Full article

Background: Vaccination is one of the most effective life-saving medical interventions, and the introduction of SARS-CoV-2 vaccines was intended to prevent the serious implications of COVID-19. The objectives of the study were (i) to observe the humoral immune response to the BNT162b2 vaccine and SARS-CoV-2 infection (mainly breakthrough infections), (ii) to demonstrate the persistence of anti-SARS-CoV-2 antibodies over time in relation to the number of received vaccine doses and the course of infection, and (iii) to determine the adverse effects after primary vaccine doses. Methods: To assess the humoral response, IgG and IgA anti-S1 antibodies were quantified by ELISA assays. In total, the tests were carried out seven times in almost two years. Results: We demonstrated strong immunogenicity (compared to levels before primary vaccination, 150- and 20-fold increases in IgG and IgA, respectively) of the BNT162b2 vaccine. Over time, we observed a systematic decline in antibody levels, which may have contributed to breakthrough infections. Although they caused seroconversion similar to the booster, antibody levels in such patients fell more rapidly than after re-vaccination. On the other hand, in individuals who did not receive booster(s) and who did not present breakthrough infection, anti-SARS-CoV-2 antibodies returned to pre-vaccination levels after 20 months. The most commonly recognized adverse effects were injection site redness and swelling. Conclusion: Vaccination is highly effective in preventing the most severe outcomes of COVID-19 and should be performed regardless of prior infection. Booster doses significantly enhance anti-SARS-CoV-2 antibody levels and, in contrast to those obtained by breakthrough infection, they remain longer. Full article