•Novel crystalline form of tartrate salt of (−)-cytisine.•Spectral analyses of the new salts cytisine tartrate (FT-IR, NMR).•Single crystal X-ray diffraction of cytisine tartrate.•Hirshfeld surface ...and 2D fingerprints plots analyses.
Why the tartrate salt of (−)-cytisine? Just because tartrate anion belongs to the group of anions that are the most often used as active pharmaceutical ingredients (APIs) of category I, according to the Orange Book, and it has been already established as a safe counterion. The salt formation is the most common and effective way for modulating physical properties of drugs and increasing solubility of potential drugs. Formation of an appropriate salt can improve the overall therapeutic and pharmaceutical effects of active pharmaceutical ingredients (APIs) in this case (−)-cytisine. The main purpose of this study was to determine the structural properties of a new cytisine salt. Cytisine is natural alkaloid and a well-known smoking cessation medication because it acts as a partial nicotinic acetylcholine receptor agonist. Because solid-state form of active pharmaceutical ingredients (APIs) can be critical for design and development of a new pharmaceutical formulation, therefore, the new salt of (−)-cytisine with L-(+)-tartaric acid was characterized using structural and spectroscopic methods: single crystal X-ray diffraction, FT-IR, 1H NMR, 13C NMR. The crystal structure is stabilized by a number of OH···−OOC, N+−H···−OOC and OH···O hydrogen bonds, in addition to van der Waals interactions. The semi-tartrate anions are joined by the strong OH⋯O hydrogen bond with an O⋯O distance of 2.502(4) Å into chains linked by one water molecule, while the other water molecule acts as a bridge between chains of the semi-tartrate anions.
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Abstract
In this study, a multivariate optimization strategy was used to develop and validate a simple, rapid, accurate, cost-effective, and stability-indicative RP-HPLC analytical method for ...quantifying hydroxychloroquine sulphate (HCQ) in coated tablets. The validation conditions involved isocratic elution mode, using a mixture of buffer solution at pH 2.2 and methanol (74:26, v/v) as the mobile phase, an Agilent® reverse phase column, model Zorbax Eclipse Plus C18 (250 cm × 4.6 mm × 5 μm), a flow rate of 1.3 mL min
−1
, column temperature 40 °C and detection at 343 nm. The method showed linearity in the range of 4–44 μg mL
−1
, with a correlation coefficient (R) of 0.9998. Recovery obtained average values of between 99.71 and 100.84% and precision with average RSD values of <2%. The robustness demonstrated by assessing the effect of seven variables (pH of the mobile phase buffer; percentage of methanol; filter brand; mobile phase flow rate; wavelength; column temperature and sample agitation time), with effect values for each variable lower than the calculated value of s√2 (1.43), showed that none of these factors had a significant influence on the analytical response. The method was applied to samples of the reference medicine Plaquinol® 400 mg and similar Reuquinol 400 mg, nomenclature established by the National Health Surveillance Agency (Anvisa), law no. 978 of 10 February 1999, purchased from local pharmacies. Results showed advantages and benefits in relation to the official method and those reported in the literature. The application of the multivariate strategy, the choice of methanol, in a lower proportion in the organic phase, due to its low toxicity, economy and easier availability compared to acetonitrile, and the other organic solvents used was a promising and important alternative for the analytical method. Furthermore, the use of reversed stationary phase, common in quality control laboratories, provided an analyte retention time of 4.595 min, demonstrating good performance and speed in routine analyses.
This study presents an electroanalytical approach to measure the catechol-O-methyltransferase (COMT) inhibitor tolcapone (TOL) using a boron-doped diamond (BDD) electrode. The application of cyclic ...voltammetry (CV) technique revealed that TOL exhibited a distinct, diffusion-controlled, irreversible anodic peak at a potential of approximately +0.71 V (vs. Ag/AgCl) in a 0.1 mol L
phosphate buffer solution (PBS) with a pH of 2.5. The oxidation of TOL is highly dependent on the pH and supporting electrolytes. Based on the data obtained from the pH investigation, a proposed mechanism for the electro-oxidation of TOL is suggested. Using the square wave voltammetry (SWV) technique, a satisfactory linear relationship was observed at approximately +0.66 V in a 0.1 mol L
PBS with a pH of 2.5. The presented method exhibited linearity within the concentration range between 1.0-50.0 μg mL
(3.7 × 10
-1.8 × 10
mol L
), with a limit of detection (LOD) of 0.29 μg mL
(1.1 × 10
mol L
). The BDD electrode demonstrated good selectivity against inorganic ions and filler materials interference. Finally, the suitability of the developed approach was assessed by measuring TOL in tablet formulations, resulting in favorable recoveries ranging from 103.4% to 106.2%.
Celotno besedilo
Dostopno za:
DOBA, IZUM, KILJ, NUK, PILJ, PNG, SAZU, SIK, UILJ, UKNU, UL, UM, UPUK
This is a cross-sectional study conducted in a veterinary pharmacy for manual production of drugs located in the city of Jo?o Pessoa, Brazil. The data collected comprised the period from January 2017 ...to December 2019, using the records system present in the pharmacy itself. We are seeing a growing demand for veterinary manipulated drugs, with a 40% increase in sales from 2017 to 2019. Among the pharmaceutical forms, capsules were the most commonly requested, followed by solutions, and among the active ingredients, itraconazole was the most frequent. With the diversity of pet species, the manipulation pharmacies have arisen to supply market needs, enabling the development of pharmaceutical forms that meet the physical characteristics of each pet species.
Introduction: Sonochemotherapy is a promising strategy for the treatment of cancer, however, there is limited understanding of its pharmacokinetics (PK).
Area covered: The PK profile of ...sonochemotherapy is evaluated based on released data. Preclinical investigations suggest that the blood PK of sonochemotherapy is similar to chemotherapy when using free anticancer drugs. When using encapsulated drugs, a lower plasma level usually occurs; however, the ultrasonic release of drugs within a tumor may lead to drugs leaking into circulation, causing a rebound in the plasma drug level; a higher drug level is detected in certain healthy organs, however this depends mostly on the pharmaceutical formulation. Sonochemotherapy increases both the level and retention time of drugs in a tumor. Clinical trials of combined chemotherapy and high intensity focused ultrasound (HIFU) are evaluated from the perspective of preclinical PK: the intratumoral PK and drug interactions under insonation, and a protocol to set the interval between drug administration and insonation are lacking.
Expert opinion: Insonation can alter the PK properties of chemotherapeutics, which may exacerbate the system and/or organ toxicity of anticancer drugs. Directly employing the PK parameters validated in conventional chemotherapy plays an important role in unsatisfactory clinical outcomes of chemotherapy combined with HIFU.
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•NMR structure of novel long acting recombinant humn insulin analog A22S-B3K-B31R established in water/acetonitrile solution•Development studies on pharmaceutical formulation are ...presented and compared to human insulin formulation.•Pharmacokinetic data are presented and compared to glargine insulin characterized by the same profile of action.
A monomer structure of a novel human insulin analog A22S-B3K-B31R (SK3R) has been characterized by NMR in water/acetonitrile solution and compared with the structure of human insulin (HIS) established in the same medium. The composition of the oligomer ensemble for neat insulins in water was qualitatively assessed by monitoring, derived from NMR experiment, translational diffusion coefficient Dix10−10m2s−1, whose value is a population averaged of individual coefficients for species in oligomeric ensemble. Nanospray ESI/MS experiment was used to establish the masses of oligomers in pharmaceutical formulation of the SK3R insulin. The pharmacodynamic data were established and compared to insulin glargine characterized by the same profile of action in diabetics. The oligomerization process of insulin during development of pharmaceutical formulation with routinely used excipients has been studied using translation diffusion coefficient Dix10−10m2s−1 established in water solution. These properties were compared with those of human insulin (HIS) which is a standard reference for novel recombinant insulins.
ENGLISH TEXT: The use of Complementary Alternative Medicine (CAM), and more specifically of Homeopathy, is common among the pediatric population in Italy. In order to verify the attitude of family ...pediatricians (pediatri di famiglia) towards the use of Homeopathy, a survey has been carried out among 5,399 (number of doctors who received the questionnaire) family pediatricians enrolled in the Italian Federation of Pediatric Physicians (Federazione Italiana Medici Pediatri, FIMP) by means of an online questionnaire. The response has been significant (1,252 questionnaires have been filled in, corresponding to 23.19% of the total submitted) and has highlighted that 29.4% of the pediatricians who took part in the survey use homeopathic medicine to cure their patients. The study has also analyzed several other parameters related to the use of Homeopathy, including age and pediatric education, most commonly treated diseases, pharmaceutical forms and possible adverse effects. ITALIAN TEXT: L’impiego delle Medicine Complementari e Alternative (Complementary Alternative Medicine, CAM), e più specificamente dell’Omeopatia, è comune tra la popolazione pediatrica in Italia. Allo scopo di verificare l’attitudine dei pediatri di famiglia nei confronti dell’utilizzo dell’Omeopatia, è stata condotta un’indagine, tramite un questionario online, tra i 5.399 (numero di medici che ha ricevuto il questionario) pediatri di famiglia appartenenti alla Federazione Italiana Medici Pediatri (FIMP). Il riscontro è stato significativo (1.252 questionari, corrispondenti al 23,19% di quelli inviati, sono stati compilati ) ed ha evidenziato che il 29,4% dei pediatri che hanno risposto all’indagine utilizza la medicina omeopatica per curare i propri pazienti. Lo studio ha anche analizzato alcuni altri parametri correlati all’impiego dell’Omeopatia, inclusi l’età e la formazione dei pediatri, le patologie più frequentemente trattate, le forme farmaceutiche utilizzate e i possibili effetti avversi.
A simple ion chromatographic (IC) method was developed and validated for simultaneous or individual determination of zoledronic, alendronic, pamidronic acids and their related substances in ...pharmaceutical formulation. The analytes were separated on Waters IC-Pak Anion HR analytical column with a nitric acid (3 mM) without any other additives, as mobile phase at a flow rate of 1.0 mL min super(-1). Inverse UV detection was used at 240 nm. Important chromatographic factors that influence the chromatography responses were screened by 11/12 Pluckett-Burman design and their interaction were assayed by 2 super(3) full factorial design. The RP-HPLC method was optimized with the aid of LC-Simulator(R) (ACD Labs, Toronto, Ontario, Canada) software. Validated method was successfully used for quantitative analysis of PAMIFOS(R), concentrate for infusion (Habitfarm AD, Ivanjica, Serbia), ZOMETA(R), powder for infusion (Novartis Pharma, Stein AG, Switzerland) and BONAP(R) tablets (Hemofarm, Vrsac, Serbia). Total chromatographic analysis time per sample was approximately 6 min, which represents significant improvement over existing methods. Validation studies revealed that the method is specific, rapid, reliable, and reproducible. Calibration plots were linear over the concentration ranges 20-120 mug mL super(-1) and 0.1-2 mug mL super(-1) for bisphosponates and their related substances, respectively. The LODs were 8.7, 4.7, 2.5, 0.026 and 0.011 mug mL super(-1) for alendronate, pamidronate, zoledronate, phosphoric acid and phosphorous acid, respectively.
The electrochemical oxidation of repaglinide has been carried out in Britton-Robinson buffer at carbon paste and glassy carbon electrodes. Repaglinide exhibits a well-defined irreversible oxidation ...peak over the entire pH range (2-11). Differential pulse voltammetry was used to determine repaglinide in pure form. The peak current varied linearly in the following ranges: 8.0×10-7-3.2×10-6 M and 4.0×10-7-4.0×10-6 M in case of carbon paste electrode and glassy carbon electrode, respectively. In case of carbon paste electrode the limits of detection (LOD) and quantification (LOQ) were 1.348×10-7 M and 4.494×10-7 M, respectively. For glassy carbon electrode the LOD and LOQ were 1.062×10-7 M and 3.54×10-7 M, respectively. The percentage recoveries were found in the following ranges: 99.09-100.07% and 99.0-100.50% for carbon paste electrode and glassy carbon electrode, respectively. The relative standard deviations were found in the following ranges: 0.636-1.395% and 0.431-1.104% in case of carbon paste electrode and glassy carbon electrode, respectively. Differential pulse voltammetry was successfully applied for the determination of repaglinide in tablets and human serum.
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