Glycosaminoglycans are carbohydrate-based compounds widely employed as nutraceuticals or prescribed drugs. Oral formulations of chondroitin sulfate combined with glucosamine sulfate have been increasingly used to treat the symptoms of osteoarthritis and osteoarthrosis. The chondroitin sulfate of these combinations can be obtained from shark or bovine cartilages and hence presents differences regarding the proportions of 4- and 6-sulfated N-acetyl β-d-galactosamine units. Herein, we proposed a systematic protocol to assess pharmaceutical batches of this combination drug. Chemical analyses on the amounts of chondroitin sulfate and glucosamine in the batches were in accordance with those declared by the manufacturers. Anion-exchange chromatography has proven more effective than electrophoresis to determine the type of chondroitin sulfate present in the combinations and to detect the presence of keratan sulfate, a common contaminant found in batches prepared with shark chondroitin sulfate. 1D NMR spectra revealed the presence of non-sulfated instead of sulfated glucosamine in the formulations and thus in disagreement with the claims declared on the label. Moreover, 1D and 2D NMR analyses allowed a precise determination on the chemical structures of the chondroitin sulfate present in the formulations. The set of analytical tools suggested here could be useful as guidelines to improve the quality of this medication.

A rapid, sensitive and simple spectrofluorimetric method was developed for the estimation of atorvastatin. In this method, the native fluorescence characteristics of atorvastatin have been studied in both acidic and basic media. High sensitivity was obtained with 5% acetic acid at 389 nm using 276 nm for excitation. Regression analysis showed a good correlation coefficient (r=0.9995) between fluorescence intensity and concentration over the range of 1.5-4 μg/mL with detection limit of 0.012 μg/mL. The proposed method was successfully applied to the analysis of atorvastatin in pure and pharmaceutical dosage forms with average recovery of 100.29±0.47%. The results were compared favorably with those of the reported method.

An isocratic sensitive and precise reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the determination and quantification of hydrocortisone in controlled-release and conventional (tablets and injections) pharmaceutical preparations. Chromatographic separation was achieved on an ODS (C18), 5 μm, 4.6 × 150 mm, with an isocratic elution using a freshly prepared mobile phase of composition methanol : water : acetic acid (60 : 30 : 10, v/v/v) at a flow rate of 1.0 ml/min. The detection of the drug was successfully achieved at a wavelength of 254 nm. The retention time obtained for the drug was 2.26 min. The proposed method produced linear detectable responses in the concentration range of 0.02 to 0.4 mg/ml of hydrocortisone. High recoveries of 98-101% were attained at concentration levels of 80%, 100%, and 120%. The intraday and interday precision (RSD) were 0.19-0.55% and 0.33-0.71%, respectively. A comparison of hydrocortisone analyses data from the developed method and the official USP method showed no significant difference (p > 0.05) at a 95% confidence interval. The method was successfully applied to the determination and quantification of hydrocortisone in six controlled-release and fifteen conventional release pharmaceutical preparations.

Selective spectrofluorometric sensing is introduced for the analysis of non-steroidal anti-androgens, darolutamide, and thalidomide in pharmaceutical preparations and biofluids. An organic fluorophore, 2,4,8,10-tetramethylpyrido[2',3':3,4]pyrazolo[1,5-a]pyrimidine 2 was synthesized in our laboratories by new simple methods to act as a fluorescent reagent for the analysis of the studied drugs. Elemental and spectral analyses were performed to approve the fluorophore structure. The fluorophore possesses a fluorescence at λem 422 nm when excited at 328 nm. The interaction between the studied drugs and the fluorophore was found to be quenching. The quenching mechanisms were studied and interpreted through the Stern-Volmer relationship. Moreover, the Stern-Volmer constants were calculated for the quenching interactions of both drugs. The introduced method was validated for the estimation of darolutamide and thalidomide in dosage forms, plasma, and urine, offering good percentage recoveries.

Endogenous Peptide Inhibitor of CXCR4 (EPI-X4) is a natural antagonist of the CXC chemokine receptor 4 (CXCR4). EPI-X4 is a 16-mer peptide that is released from human serum albumin (HSA) by acidic aspartic proteases such as Cathepsin D and E. Since human serum albumin (HSA) is an important medicinal substance we asked whether different pharmaceutical HSA products contain EPI-X4 which could have been generated during manufacturing and whether HSA can serve as a substrate for cathepsins despite of the presence of stabilizers like caprylate.

The aim of this study was to develop and validate a simple, sensitive, precise and cost-effective one-level agar diffusion (5+1) bioassay for estimation of potency and bioactivity of Levofloxacin in pharmaceutical preparation which has not yet been reported in any pharmacopoeia. Among 16 microbial strains, Bacillus pumilus ATCC-14884 was selected as the most significant strain against Levofloxacin. Bioassay was optimized by investigating several factors such as buffer pH, inoculums concentration and reference standard concentration. Identification of Levofloxacin in commercial sample Levoflox tablet was done by FTIR spectroscopy. Mean potency recovery value for Levofloxacin in Levoflox tablet was estimated as 100.90%. A validated bioassay method showed linearity (r2=0.988), precision (Interday RSD=1.05%, between analyst RSD=1.02%) and accuracy (101.23%, RSD=0.72%). Bioassay was correlated with HPLC using same sample and estimated potencies were 100.90% and 99.37%, respectively. Results show that bioassay is a suitable method for estimation of potency and bioactivity of Levofloxacin pharmaceutical preparations.

The aim of the present study was to investigate if patterns obtained from evaporating droplets of pharmaceutical preparations reveal the impact of succussion on such medicinal products. For this purpose, five pharmaceutical preparations (Echinacea 10-2, Baptisia 10-3, Baptisia 10-4, Luffa 10-4, and Spongia 10-6) were prepared according to the European Pharmacopoeia guidelines for the production of homeopathic remedies, in three variants each: with varying numbers of succussion strokes (i) 100, (ii) 10 (succussed samples), and (iii) zero (gently mixed, unsuccussed sample). System stability was studied by means of systematic positive control experiments. Patterns were evaluated by means of computerized image analysis regarding grey level distribution, texture, and fractality. For all investigated pharmaceutical preparations, significant differences were found between the succussed and gently mixed samples; whereas, all three samples (prepared with 100, 10 and zero succussion strokes) could be significantly differentiated for Luffa 10-4 and Spongia 10-6 for one image evaluation parameter each. Control experiments showed a reasonable stability of the experimental set-up.

This paper describes a procedure that has been optimized for the determination of lamotrigine by Differential Pulse Adsorptive Stripping Voltammetry (DPAdSV) using carbon screen-printed electrodes (CSPE) and mercury coated carbon screen-printed electrodes. Selection of the experimental parameters was made using experimental design methodology. The detection limit found was 5.0 x 10-6 M and 2.0 x 10-6 M for the non modified and Hg modified CSPE, respectively. In terms of reproducibility, the precision of the above mentioned methods was calculated in %RSD values at 9.83% for CSPE and 2.73% for Hg-CSPE. The Hg-coated CSPEs developed in this work were successfully applied in the determination of lamotrigine in pharmaceutical preparations.

The discovery of new solutions with antibacterial activity as efficient and safe alternatives to common preservatives (such as parabens) and to combat emerging infections and drug-resistant bacterial pathogens is highly expected in cosmetics and pharmaceutics. Colloidal silver nanoparticles (NPs) are attracting interest as novel effective antimicrobial agents for the prevention of several infectious diseases.

Naproxen is one of the most used non-steroidal anti-inflammatory drugs (NSAIDs). It is used to treat pain of various origins, inflammation and fever. Pharmaceutical preparations containing naproxen are available with prescription and over-the-counter (OTC). Naproxen in pharmaceutical preparations is used in the form of acid and sodium salt. From the point of view of pharmaceutical analysis, it is crucial to distinguish between these two forms of drugs. There are many costly and laborious methods to do this. Therefore, new, faster, cheaper and, at the same time, simple-to-perform identification methods are sought. In the conducted studies, thermal methods such as thermogravimetry (TGA) supported by calculated differential thermal analysis (c-DTA) were proposed to identify the type of naproxen in commercially available pharmaceutical preparations. In addition, the thermal methods used were compared with pharmacopoeial methods for the identification of compounds, such as high-performance liquid chromatography (HPLC), Fourier-transform infrared spectroscopy (FTIR), UV-Vis spectrophotometry, and a simple colorimetric analyses. In addition, using nabumetone, a close structural analog of naproxen, the specificity of the TGA and c-DTA methods was assessed. Studies have shown that the thermal analyses used are effective and selective in distinguishing the form of naproxen in pharmaceutical preparations. This indicates the potential possibility of using TGA supported by c-DTA as an alternative method.

A novel potentiometric ion-selective PVC membrane sensor for analysis of atorvastatin (AT) in pharmaceutical preparations based on atorvastatin-(tetraphenyl borate), (AT-(TPB)2) as sensing element, tetraphenyl borate as additive and tris-2-ethyl-hexyl phosphate (TOP) as plasticizer solvent was prepared. The electrode shows a good Nernestian response over the concentration range of 0.09-5586 μg mL(-1)of AT with slope of 30.1±0.1 mV/decade and limit of detection0.056μg mL(-1).The response time of sensor is fats (less than 10 sec) and could be used for about one month in the pH range of 4.5-8.0. The electrode exhibit good selectivity for the AT in the presence of large amount of co-drugs and inorganic cations. The method is precise and accurate with mean relative standard deviation of <2%.Atorvastatin is determined successfully in several tablets by the proposed membrane.

Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations.

Pressure ulcers often become chronic wounds that are difficult to treat and that tend to recur after healing. In China, convincing data from randomised trials have demonstrated that the pharmaceutical preparations of Periplaneta americana (KangFuXin Liquid, KFX) have a significant efficacy for pressure ulcers. To provide more reference to the clinicians and experts, we conducted a meta-analysis based on the existing randomised controlled trials (RCTs). We searched the RCTs about KFX for the treatment of pressure ulcers published up to July 2022 in major English and Chinese databases with no language restriction, including PubMed, EMBASE, Web of Science (WOS), Cochrane Central Register of Controlled Trials (CENTRAL), China Network Knowledge Infrastructure (CNKI), Chinese Biomedicine (CBM), Chinese Scientific Journals Database (VIP), and WanFang database. Cochrane Handbook guidelines were used to assess the risk of bias and to evaluate the methodological quality of included RCTs. Estimates of the intervention's effects are expressed as the risk ratio (RR) (95% CI) for binary outcomes and mean difference or standardised mean difference (95% CI) for continuous outcomes. We applied fixed or random effects models, and all analyses were performed using Review Manager version 5.4 and Stata/SE version 12.0. We included 22 studies with a total of 1575 participants. Compared with controls, KFX combined with basic wound care or KFX combined with basic wound care and another topical drug or physical treatment significantly increase clinical efficacy (RR: 1.17; 95% CI, 1.06-1.28; P = 0.001; I2  = 81%) and shorten the complete healing time (MD = -5.11; 95% CI [-8.19, -2.02]; P = 0.001) for pressure ulcers. Subgroup analysis showed a significant difference in the total clinical effect rate between KFX combined with basic wound care and controls. (n = 1018, RR 1.21, 95% CI [1.07, 1.36], I2  = 82%, P = 0.003). No difference was found in the total clinical effective rate between patients using KFX combined with basic wound care and another topical drug or physical treatment with controls (KFX combined with basic wound care and topical physical treatment: n = 267, RR 1.15, 95% CI [0.86, 1.52], I2  = 87%, P = 0.34; KFX combined with basic wound care and topical drug: n = 290, RR 1.05, 95% CI [0.80, 1.37], I2  = 86%, P = 0.71). Based on treatment duration, subgroup analysis indicated that increasing treatment duration increased the total clinical effective rate when treatment duration was not long. (treatment duration: 14 days: n = 158, OR 5.48, 95% CI [1.47, 20.43], I2  = 0%, P = 0.01; 21 days: n = 132, OR 5.93, 95% CI [1.86, 18.91], I2  = 65%, P = 0.003). When treatment duration was 28 days or 30 days, the results showed that there was no significant difference in total clinical effective rate between interventions and controls (treatment duration: 28 days: n = 107, OR 3.04, 95% CI [0.25, 37.32], I2  = 50%, P = 0.38; 30 days: n = 256, OR 0.58, 95% CI [0.11, 3.15], I2  = 65%, P = 0.53). No data on side effects were reported in any of the 22 studies. The conclusion is that the combination of KFX and basic wound care is effective in increasing the total clinical effectiveness and shortening the complete healing time of pressure ulcers.

The goal of elimination of the human filariases would benefit greatly from the use of a macrofilaricidal agent. In vivo trials in humans and many experimental animal models suggest that flubendazole (FLBZ) is a highly efficacious macrofilaricide. However, since serious injection site reactions were reported in humans after parenteral FLBZ administration, the search for alternative pharmaceutical strategies to improve the systemic availability of FLBZ and its metabolites has acquired urgency in both human and veterinary medicine. The goal of the current work was to compare the systemic exposure of FLBZ formulated as either an aqueous hydroxypropyl-β-cyclodextrin (CD) or aqueous carboxymethyl cellulose (CMC) suspension or a Tween 80-based formulation (TWEEN) in rats and jirds (Meriones unguiculatus). Healthy animals of both species were allocated into four experimental groups of 44 animals each: FLBZ-CD oral and FLBZ-CDsc, treated with the FLBZ-CD formulation by the oral or subcutaneous routes, respectively; FLBZ-TWEENsc, dosed subcutaneously with the FLBZ-TWEEN formulation; and FLBZ-CMC oral, treated orally with the FLBZ suspension. The FLBZ dose was 5 mg/kg. FLBZ and its hydrolyzed (H-FLBZ) and reduced (R-FLBZ) metabolites were recovered in plasma samples collected from rats and jirds treated with the different FLBZ formulations. In both species, FLBZ parent drug was the main analyte recovered in the bloodstream. In rats, FLBZ systemic exposure (AUC 0-LOQ) was significantly (P < 0.05) higher after the FLBZ-CD treatments, both oral (4.8 ± 0.9 µg.h/mL) and subcutaneous (7.3 ± 0.6 µg.h/mL), compared to that observed after oral administration of FLBZ-CMC suspension (0.93 ± 0.2 µg.h/mL). The same differences were observed in jirds. In both species, parenteral administration of FLBZ-TWEEN did not improve the systemic availability of FLBZ compared to FLBZ-CDoral treatment. In conclusion, formulation approaches that enhance the availability of flubendazole in the rat and jird may have therapeutic implications for a drug with poor or erratic bioavailability.

A new, simple and repeatable liquid chromatography method with charged aerosol detection (LC-CAD) for the determination of gentamicin sulphate composition and related substances has been developed. Gentamicin lacks of chromophores, therefore its determination is quite problematic. Using a universal CAD enables to achieve good separation without sample derivatization. Mass spectrometry was employed to confirm the LC-CAD peak profile. The proposed method was validated and applied for the determination of gentamicin sulphate composition and related substances in pharmaceutical preparations.

This article is focused on the determination of lidocaine hydrochloride as a local anaesthetic drug. A potentiometric method based on modified screen-printed and modified carbon paste ion-selective electrodes was described for the determination of lidocaine hydrochloride in different pharmaceutical preparations and biological fluids (urine and serum). It was based on potentiometric titration of lidocaine hydrochloride using modified screen-printed and carbon paste electrodes as end point indicator sensors. The influences of the paste composition, different conditioning parameters and foreign ions on the electrodes performance were investigated and response times of the electrodes were studied. The electrodes showed Nernstian response of 58.9 and 57.5 mV decade-1 in the concentration range of 1×10-7-1×10-2 and 6.2×10-7-1×10-2 mol L-1 for modified screen-printed and carbon paste electrodes, respectively. The electrodes were found to be usable within the pH range of 2.0-8.0 and 2.0-7.5, exhibited a fast response time (about 6 and 4) low detection limit (1×10-7 and 6.2×10-7 mol L-1), long lifetime (6 and 4 months) and good stability for modified screen-printed (Electrode VII) and carbon paste electrodes (Electrode III), respectively. The electrodes were successfully applied for the determination of lidocaine hydrochloride in pure solutions, pharmaceutical preparation and biological fluids (urine and serum) samples. The results obtained applying these potentiometric electrodes were comparable with British pharmacopeia. The method validation parameters were optimized and the method can be applied for routine analysis of lidocaine hydrochloride drug.

Carbon quantum dots (CQDs) are new class of carbon nanoparticles. Recently, they have been widely used as fluorescent probes due to their easy accessibility, optical properties and chemical inertness. Many available precursors are used in the synthesis of carbon quantum dots. The electrical and optical properties of CQDs could be enhanced by doping hetero atoms such as nitrogen or sulfur into their structure.

The use of cannabis flowering tops with standardized amounts of active phytocannabinoids was recently authorized in several countries to treat several painful pathological conditions. The acute pharmacological effects and disposition of Δ-9-tetrahydrocannabinol (THC), cannabidiol (CBD), their acidic precursors and THC metabolites after oil and decoction administration have been already described. In this study, the disposition of CBD metabolites: 7-carboxy-cannabidiol (7-COOH-CBD), 7-hydroxycannabidiol (7-OH-CBD), 6-α-hydroxycannabidiol (6-α-OH-CBD), and 6-β-hydroxycannabidiol (6-β-OH-CBD) in the serum and urine of healthy volunteers was presented. Thirteen healthy volunteers were administered 100 mL of cannabis decoction in the first experimental session and, after 15 days of washout, 0.45 mL of oil. Serum and urine samples were collected at different time points, and the CBD metabolites were quantified by ultra-high-performance liquid chromatography-tandem mass spectrometry. The most abundant serum metabolite was 7-COOH-CBD, followed by 7-OH-CBD, 6-β-OH-CBD, and6-α-OH-CBD, after decoction and oil. Both 7-OH-CBD and the 6-α-OH-CBD showed similar pharmacokinetic properties following administration of both cannabis preparations, whereas 7-COOH and 6-α-OH-CBD displayed a significant higher bioavailability after decoction consumption. All CBD metabolites were similarly excreted after oil and decoction intake apart from 6-α-OH-CBD, which had a significantly lower excretion after oil administration. The pharmacokinetic characterization of CBD metabolites is crucial for clinical practice since the cannabis herbal preparations are increasingly used for several pathological conditions.

A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV) was described. In this method, all selenium spices reduced to selenium (IV) using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV) in aqueous solution. The proposed method is based on the complexation of Selenium (IV) with dithizone at pH < 1 in micellar medium (Triton X-100). After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm) and dithizone (434 nm) overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL(-1); the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL(-1) of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples.

In this work, an automated flow injection analysis (FIA) connected to a boron-doped diamond electrode (BDDE) was originally developed for the analysis of methimazole in pharmaceutical preparations. At a modification-free BDDE, methimazole was easilly oxidized. For the analysis of the mechanisms occurring at the electrode surface, cyclic voltammetry was employed to evaluate the impact of fundamental experimental parameters, such as pH and scan rate, on the BDDE response. For the quantitative detection, the FIA amperometric approach was constructed and used as a fast and sensitive method. The suggested approach provided a broad linear range of 0.5-50 μmol/L and a low detection limit of 10 nmol/L (signal-to-noise ratio = 3). Furthermore, the BDDE was successfully utilized to quantify methimazole in genuine samples from a variety of medicines, and its performance remained steady after more than 50 tests. The findings of amperometric measurements exhibit excellent repeatability, with relative standard deviations of less than 3.9 and 4.7 % for intra-day and inter-day, respectively. The findings indicated that, compared with traditional approaches, the suggested method has the following advantages: quick analysis time, simplicity, highly sensitive output, and no need for complicated operational processes.