GAS CHROMATOGRAPHIC DETERMINATION OF METHYLSULFONYLMETHANE IN AN ANTI-ARTHRITIC COMBINED PHARMACEUTICAL PRODUCT Andrii Koptielov, Volodymyr Petruk, Olena Bevz, Olha Rudakova, Oleksandr Kryvanych, et al. Sciencerise Pharmaceutical Science, 2026 Methylsulfonylmethane is a pharmacologically active compound that is widely used in mono- and combined pharmaceutical preparations to maintain the functional state of the musculoskeletal system. The development of promising anti-arthritic drugs requires proper analytical support, particularly the use of validated methods suitable for routine quality control in accordance with modern pharmaceutical requirements.The aim. The aim of the study was to develop and validate methods for the quantitative determination of methylsulfonylmethane in a combined medicinal product using gas chromatography with mass-selective detection (GC-MS) and flame ionization detection (GC-FID), and to compare their validation characteristics.Materials and methods. The object of the study was a combined medicinal product in the form of a powder containing methylsulfonylmethane, glucosamine sulfate, chondroitin sulfate sodium and excipients. The study was conducted using Shimadzu GC/MS GCMS-QP2020 EI and Shimadzu GC-2010 Plus AF gas chromatographs with a flame ionization detector using capillary columns of type 5MS and the external standard method. The validation of the methods was carried out in accordance with the requirements of the State Pharmacopoeia of Ukraine and ICH Q2(R1) recommendations.Results. Two methods for the identification and quantitative determination of methylsulfonylmethane by gas chromatography were developed. The retention time of MSM by the GC-MS method was 9.157 min in the reference solution and 9.163 min in the test solution, and by the GC-FID method - 8.456 and 8.442 min, respectively. The validation characteristics of the methods were confirmed in the range of 80–120% of the nominal content (0.32–0.48 mg/ml) with correlation coefficients r > 0.9981. The relative standard deviations did not exceed 0.42%, and the total analytical uncertainty met the pharmacopoeial acceptance criteriaConclusions. The proposed methods are accurate, reproducible and suitable for routine quality control of combination medicinal products containing methylsulfonylmethane
Prospects for off-label use of propranolol for the treatment of infantile hemangioma in children I.O. Surzhykov, O.V. Bevz, V.A. Goncharuk, O.V. Kryvanych, N.Y. Bevz, et al. Medicni Perspektivi, 2025 Infantile hemangiomas are the most common benign vascular tumors in infants, with a detection rate of 2-5% in newborns, while among premature infants their incidence reaches 23%. These tumors can vary greatly in size and location, sometimes causing serious complications such as visual, respiratory or bleeding disorders, which significantly impair the quality of life of patients and can lead to long-term consequences. Propranolol in the form of an oral solution has been approved as a first-line treatment for infantile hemangiomas, it has vasoconstrictor and antiangiogenic effects and promotes the induction of apoptosis of tumor endothelial cells, resulting in a significant reduction in hemangioma size and improvement in patient condition. Despite the high incidence of the disease, there are no standardized propranolol medicines for pediatric patients in Ukraine, which greatly complicates treatment and forces doctors to use off-label drugs. This creates risks associated with improper dosage, variability in the concentration of the active ingredient, and possible side effects. The purpose of the study is to analyze the scientific literature on the efficacy and safety of propranolol in the treatment of infantile hemangiomas, as well as to justify the need to develop new dosage forms for pediatrics. To achieve this goal, we analyzed scientific articles, clinical trial data, and the legislative framework, including international guidelines and treatment protocols. The study used methods of analysis, information systematization and genera¬lization.The results of the study show that propranolol is highly effective in the treatment of hemangiomas. Its therapeutic effect is explained by vasoconstrictor, antiangiogenic effects and induction of apoptosis of tumor endothelial cells. According to clinical trials, the standard treatment regimen involves the use of propranolol at a dose of 2-3 mg/kg of body weight per day for six months, which helps to reduce tumor size, low the possibility of complications and improve the quality of life of patients. The development of new, standardized pharmaceutical products for children with propranolol will increase the effectiveness of treatment and minimize side effects, making this issue relevant for both clinical practice and the pharmaceutical industry.
DETERMINATION OF CHROMATOGRAPHIC CONDITIONS FOR QUANTITATIVE ASSESSMENT OF ACTIVE COMPONENTS IN COMPLEX NASAL SPRAY AFTER MANUFACTURING AND EXPIRY DATE Valeriia Cherniakova, Artem Myhal, Vitalii Rudiuk, Oleksandr Kryvanych, Olha Rudakova, et al. Sciencerise Pharmaceutical Science, 2024 The aim of the work is the development of chromatographic conditions, the study of the validation characteristics of the method of quantitative determination of phenylephrine hydrochloride, nitrofural, lidocaine hydrochloride and diphenhydramine hydrochloride, panthenol, povidone in the joint presence in the nasal spray by a complex method of liquid chromatography with UV detection. Evaluation of the quantitative content of active components after manufacturing and during the shelf life.Materials and methods. Agilent 1260 liquid chromatographs, equipped with a diode-matrix detector from the company "Agilent technologies", USA. Chromatographic columns 250×4.6 mm in size, filled with octadecylsilyl silica gel for chromatography (Zorbax StableBond SB-Aq, Agilent company), mobile phase A - phosphate buffer solution pH 7.0 - acetonitrile P (1650:350), mobile phase B – acetonitrile P; elution mode – gradient; mobile phase flow rate – 1.0 ml/min; detection wavelengths – 220 nm (for panthenol, phenylephrine, povidone, diphenhydramine) and 235 nm (for nitrofural and lidocaine).Results. Chromatographic separation conditions were developed for the co-presence determination of six target substances: panthenol, phenylephrine hydrochloride, nitrofural, povidone, lidocaine hydrochloride and diphenhydramine hydrochloride. The suitability of the technique for this task was confirmed by determining the validation characteristics. The methodology at the appropriate level is characterized by specificity, linearity, correctness and convergence in the range of application for panthenol (range 20.33-38.26 mg/ml, ΔZ=0.93 ≤ max ΔZ=3.20, a=0.63 max a=5.12, r = 0.9978 min r= 0.9924), phenylephrine hydrochloride (range 1,70-3,21 mg/ml, ΔZ=0.51 ≤ max ΔZ=3.20, a=0.15 max a=5.12, r = 0.9984 min r= 0.9924), nitrofural (range 0.137-0.257 mg/ml, ΔZ=0.91 ≤ max ΔZ=3.20, a=0.032 max a=5.12, r = 0.9987 min r= 0.9924) povidone (range 20,44-38,50 mg/ml, ΔZ=0.23 ≤ max ΔZ=3.20, a=2,33 max a=5.12, r = 0.9942 min r= 0.9924), lidocaine hydrochloride (range 6,80-12,81 mg/ml, ΔZ=0.34 ≤ max ΔZ=3.20, a=0.66 max a=5.12, r = 0.9988 min r= 0.9924), diphenhydramine hydrochloride (range 1,36-2,56 mg/ml, ΔZ=0.20 ≤ max ΔZ=3.20, a=0.15 max a=5.12, r = 0.9980 min r= 0.9924). There are no significant changes when stored at 25 °C for 6 months.Conclusions. An analytical method of quantitative determination of the component composition in an extemporaneous nasal spray by a complex method of high-performance liquid chromatography has been developed. The determined validation parameters confirm the correctness of the methodology. The chemical stability of the dosage form is observed for 6 months
DESIGN AND VALIDATION OF ANALYTICAL METHODS FOR QUANTITATIVE DETERMINATION OF ACTIVE INGREDIENTS IN EXTEMPORAL COMBINED MEDICINE IN SPRAY FORM Valeriia Cherniakova, Artem Myhal, Vitalii Rudiuk, Yaroslav Studenyak, Oleksandr Kryvanych, et al. Sciencerise Pharmaceutical Science, 2023 The aim of the work was the development and study of the validation characteristics of the method of quantitative determination of phenylephrine hydrochloride, nitrofural and diphenhydramine hydrochloride when they are simultaneously present in an extemporaneous combined medicinal product in the form of a spray using liquid chromatography method.Materials and methods. Agilent 1260 liquid chromatographs, equipped with a diode-matrix and UV detector from the company "Agilent technologies", USA. Chromatographic columns 250×4.6 mm filled with octadecylsilyl silica gel for chromatography (Zorbax StableBond SB-Aq, Agilent company), mobile phase - 0.1 % aqueous solution of trifluoroacetic acid R - methanol R, elution mode - gradient; mobile phase speed – 1.2 ml/min; the detection wavelength is 220 nm.Results. The determined chromatographic conditions ensure proper separation of the peaks of the substances to be determined: phenylephrine hydrochloride, nitrofural and diphenhydramine hydrochloride in their joint presence, and do not have a negative effect on the quantitative assessment of their content. Validation tests were conducted to confirm the suitability of the analytical method for the performance of the task - control of the quantitative content of active substances in the combined medicinal product in the form of a spray. The determined validation characteristics indicate that the method is characterized by appropriate specificity, linearity, correctness and convergence in the range of application for phenylephrine hydrochloride (range 0.499-0.749 mg/ml, ΔZ=0.44 ≤ max ΔZ=3.20, d=0.22 ≤ max d=1.02, a=0.01 max a=5.1, r = 0.9997 min r= 0.9924), nitrofural (range 0.154-0.231 mg/ml, ΔZ=0.44 ≤ max ΔZ=3.20, d=0.62 ≤ max d=1.02, a=0.0006 max a=5.1, r = 0.9996 min r= 0.9924) and diphenhydramine hydrochloride (range 0.499-0.749 mg/ml, ΔZ=0.50 ≤ max ΔZ=3.20, d=0.05 ≤ max d=1.02, a=0.076 max a=5.1, r = 0.9999 min r= 0.9924).Conclusions. An analytical technique for the quantitative determination of phenylephrine hydrochloride, nitrofural and diphenhydramine hydrochloride when simultaneously present in an extemporaneous combined medicinal product in the form of a spray by the method of high-performance liquid chromatography was developed. The determined validation parameters confirm the correctness of the methodology. The proposed HPLC technique was used to study the chemical stability of the spray for the treatment of allergic rhinitis
