Pharmaceutical Formulations Research Articles

Evaluation of the Greenness, Whiteness, and blueness profiles of stability indicating HPLC method for determination of Denaverine hydrochloride and benzyl alcohol in pharmaceuticals

Recently, there has been important emphasis in pharmaceutical analysis on the stability of drug formulations and the development of appropriate stability-indicating studies. In this regard, a comprehensive stability-illustrating RP-HPLC approach has been established and validated for the assay of denaverine hydrochloride (DEN) and benzyl alcohol (BNZ) in Sensiblex® Injectable Solution.Different stress conditions were applied to both components, following the guidelines of the International Conference on Harmonization (ICH). Using the isocratic elution technique, DEN, BNZ, and their degradation products were effectively isolated and quantified on an Inertsil C8 column at room temperature. The mobile phase consisted of acetonitrile: water: orthophosphoric acid (80:20:0.1, by volume), and the flow speed was maintained at 0.8 mL/min. Detection was performed at 220 nm using a diode array detector, with concentration ranges of 10.00–30.00 and 5.00–15.00 μg/mL for DEN and BNZ, respectively. The total analysis time was less than five minutes, establishing this novel chromatographic method as a priority for routine quality control analysis of both drugs. The inclusion of acetonitrile was necessary for achieving adequate resolution. The environmental impact was evaluated using three approaches: Green Analytical Procedure Index (GAPI), Analytical Eco-Scale, and Analytical GREEnness metric (AGREE). Additionally, White Analytical Chemistry (WAC) was employed to evaluate the quality (R), ecological impact (G), and economic viability (B) of the developed approach.Additionally, the newly presented Blue Applicability Grade Index (BAGI) metric was also assessed. The final Eco-scale score of 85 and the AGREE score of 0.65 indicate the environmentally friendly nature of the new chromatographic method. The BAGI final score was 82.5, while the overall score of the WAC tool was 91.8, highlighting the method's practicality and utility. DEN exhibits the highest degradation (24%) in acidic conditions, whereas BNZ is particularly susceptible to oxidative degradation, with a degradation percentage of 35%. New four degradation products were formed, and the two investigated compounds were efficiently separated and analyzed in their presence. Further identification of degradation products for DEN and BNZ is strongly recommended, employing a mass spectrophotometric detector. Notably, the novel method is accurate, reliable, economical, and time-efficient. In conclusion, it can be effectively employed for routine quality control and stability assessment of DEN and BNZ in both their pure form and pharmaceutical formulations.

Hydrophilic Interaction Liquid Chromatography for the Analysis of Pharmaceutical Formulations

Abstract: For a long time, Reversed-Phase Liquid Chromatography (RPLC) was the most dominant technique for the analysis of pharmaceutical compounds, but with poor efficiency in the separation of small polar molecules. From the efforts to solve the problem of insufficient retention of these molecules, during the last decades, a mode of liquid chromatography named Hydrophilic Interaction Liquid Chromatography (HILIC) has experienced vast expansion. It is based on the use of a highly hydrophilic stationary phase along with an aqueous mobile phase with high organic modifier content. In this review, the characteristics of stationary and mobile phases used in HILIC are described, and corresponding separation mechanisms are discussed. An overview of recently published papers dealing with the application of HILIC in analyzing pharmaceuticals in biological and non-biological samples is provided. Besides, the application of HILIC systems in the determination of the physicochemical properties of compounds is described.

Preparation, Physicochemical Characterization, and Stability Study of Lippia origanoides Essential Oil-Based Nanoemulsion as a Topical Delivery System.

Fungal diseases are a priority in research, development, and health care, according to the WHO, mainly due to Candida spp. Essential oils (EOs) of the genus Lippia have demonstrated broad antimicrobial biological activity. Previous studies identified the anti-Candida potential of a thymol/p-cymene chemotype EO from Lippia origanoides H.B.K coded "0018". Nanoemulsions favor the biological activity of EOs and overcome limitations such as low solubility, instability against oxidizing agents, pH, light, and low permeability. To develop, characterize, and adjust a prototype of an O/W nanoemulsion containing the "0018" EO from Lippia origanoides for its evaluation in an In vitro permeability study. Nanoemulsions were obtained using a high energy high shear method. Their particle size distribution, Z potential, viscosity, pH, encapsulation efficiency (EE), thermodynamic stability and the Turbiscan Stability Index (TSI) were evaluated. The nanoemulsion prototype was adjusted to improve performance characteristics and microbiological efficacy. Thymol was used as an analyte in the EO quantification using UHPLC-DAD. An O/W nanoemulsion with hydrodynamic diameter <200 nm and polydispersity index <0.3, EE >95%, with TSI < 1.5, anti-Candida albicans efficiency >95% was obtained; permeable with a flow of 6.0264 µg/cm2/h and permeability coefficient of 1.3170x10-3 cm/h. A pharmaceutical formulation prototype is obtained that maintains the physical and physicochemical characteristics over time. Permeability is verified in an in-vitro model. It is proposed to evaluate its antifungal activity in preclinical or clinical studies as a contribution to the treatment of topical fungal diseases caused by Candida spp., through the use of biological resources and Colombian biodiversity.

Floating drug delivery systems: A review

To boost medication bioavailability, target the stomach mucosa, and lengthen gastric residence time, a multi-unit oral floating drug delivery system was created. Due to their potential to enhance drug delivery, floating tablets have become more significant in pharmaceutical formulation. In the upper GIT, where the environment is acidic, tablets absorbs poorly. The bioavailability shows 50% when administer orally. An H2-receptor antagonist called tablets is frequently prescribed to treat gastrointestinal issues brought on by excess stomach acid. With the right excipients and polymers, floating tablets are meant to float on the contents of stomach Over an extended length of time, extending medication release and bioavailability. This review examines the advantages, disadvantages, and in vitro or in-vivo evaluation of famotidine floating tablets with an emphasis on their potential to improve treatment outcomes and patient compliance.

Phase-sensitive Optical Coherence Tomography reveals droplet penetration into a powder bed

Understanding the mixing behavior that unfolds when liquid droplets impact on powder beds requires a sub-surface dynamic imaging method that provides high spatial and temporal resolution. In this study, a high-resolution phase-sensitive optical coherence tomography (PhS-OCT) technique was introduced to provide in-depth insights into the interaction of droplets and powder beds. A theoretical model correlating changes in the optical path differences (OPD) of the OCT signal with physical properties of the powder bed was presented. Experiments were conducted on three powders with median particle diameters, i.e., the size corresponding to the 50th percentile of the cumulative volume distribution, of 3 µm (mannitol), 4 µm (mannitol) and 109 µm (SV010). Water and ethanol droplets were used to illustrate the technique. The results demonstrated that OPD maps can qualitatively resolve the liquid-powder mixture region, both temporally and spatially, as the droplet diffuses into the powder bed, allowing for a quantitative description of diffusion behavior. A comparison of lactose and mannitol powder samples revealed varying diffusion rates, potentially attributed to differences in porosity, particle size, and agglomeration. Additionally, water and ethanol droplets exhibited significantly different (p = 0.005) diffusion profiles for the same powder properties. In general, the findings indicate the potential of the proposed PhS-OCT technique for evaluating the mixing behavior of multi-phase mixtures, holding promise in applications such as pharmaceutical drug formulations and additive manufacturing.

New Generation Nebulizers.

Standard nebulizers are intended for general purpose use and typically are continuously operated jet or ultrasonic nebulizers. Evolutionary developments such as breath-enhanced and breath-triggered devices have improved delivery efficiency and ease of use, yet are still suitable for delivery of nebulized medications approved in this category. However, recent developments of vibrating membrane or mesh nebulizers have given rise to a significant increase in delivery efficiency requiring reformulation of former drug products or development of new formulations to match the enhanced delivery characteristics of these new devices. In addition, the electronic nature of the new devices enables tailoring to specific applications and patient groups, such as guiding or facilitating optimal breathing and improving adherence to the therapeutic regimen. Addressing these patient needs leads to new nebulization technologies being embedded in devices with fundamentally distinct functionality, modes of operation and patient interfaces. Therefore, new generation nebulizers can no longer be regarded as one category with fairly similar performance characteristics but must be clinically tested and approved as drug/device combinations together with the specific drug formulation, similar to the approval of pressurized metered-dose inhalers and dry powder inhalers. From a regulatory viewpoint, it is required that drug and device are associated with each other as combinations by clear, mutually conforming labels or, even more desirably, by distinct container-closure systems (closed system nebulizer).

SCARLET (Supplemental Citicoline Administration to Reduce Lung injury Efficacy Trial): study protocol for a single-site, double-blinded, placebo-controlled, and randomized Phase 1/2 trial of i.v. citicoline (CDP-choline) in hospitalized SARS CoV-2-infected patients with hypoxemic acute respiratory failure

BackgroundThe SARS CoV-2 pandemic has resulted in more than 1.1 million deaths in the USA alone. Therapeutic options for critically ill patients with COVID-19 are limited. Prior studies showed that post-infection treatment of influenza A virus-infected mice with the liponucleotide CDP-choline, which is an essential precursor for de novo phosphatidylcholine synthesis, improved gas exchange and reduced pulmonary inflammation without altering viral replication. In unpublished studies, we found that treatment of SARS CoV-2-infected K18-hACE2-transgenic mice with CDP-choline prevented development of hypoxemia. We hypothesize that administration of citicoline (the pharmaceutical form of CDP-choline) will be safe in hospitalized SARS CoV-2-infected patients with hypoxemic acute respiratory failure (HARF) and that we will obtain preliminary evidence of clinical benefit to support a larger Phase 3 trial using one or more citicoline doses.MethodsWe will conduct a single-site, double-blinded, placebo-controlled, and randomized Phase 1/2 dose-ranging and safety study of Somazina® citicoline solution for injection in consented adults of any sex, gender, age, or ethnicity hospitalized for SARS CoV-2-associated HARF. The trial is named “SCARLET” (Supplemental Citicoline Administration to Reduce Lung injury Efficacy Trial). We hypothesize that SCARLET will show that i.v. citicoline is safe at one or more of three doses (0.5, 2.5, or 5 mg/kg, every 12 h for 5 days) in hospitalized SARS CoV-2-infected patients with HARF (20 per dose) and provide preliminary evidence that i.v. citicoline improves pulmonary outcomes in this population. The primary efficacy outcome will be the SpO2:FiO2 ratio on study day 3. Exploratory outcomes include Sequential Organ Failure Assessment (SOFA) scores, dead space ventilation index, and lung compliance. Citicoline effects on a panel of COVID-relevant lung and blood biomarkers will also be determined.DiscussionCiticoline has many characteristics that would be advantageous to any candidate COVID-19 therapeutic, including safety, low-cost, favorable chemical characteristics, and potentially pathogen-agnostic efficacy. Successful demonstration that citicoline is beneficial in severely ill patients with SARS CoV-2-induced HARF could transform management of severely ill COVID patients.Trial registrationThe trial was registered at www.clinicaltrials.gov on 5/31/2023 (NCT05881135).Trial statusCurrently enrolling.

Genomics and transcriptomics reveal β-carotene synthesis mechanism in Dunaliella salina

Dunaliella salina is by far the most salt-tolerant organism and contains many active substances, including β-carotene, glycerol, proteins, and vitamins, using in the production of dried biomass or cell extracts for the biofuels, pharmaceutical formulations, food additives, and fine chemicals, especially β-carotene. We report a high-quality genome sequence of D. Salina FACHB435, which has a 472 Mb genome size, with a contig N50 of 458 Kb. A total of 30,752 protein-coding genes were predicted. The annotation results evaluated by BUSCO was shown that completeness was 91.0% and replication was 53.1%. The fragments were 6.3% and the deletions were 2.6%. Phylogenomic and comparative genomic analyses revealed that A. thaliana diverged from Volvocales about 448 million years ago, then Volvocales C. eustigma, D. salina, and other species diverged about 250 million years ago. High light could promote the accumulation of β-carotene in D. salina at a 13 d stage of culture. The enrichment of DEGs in KEGG, it notes that the predicted up-regulated genes of carotenoid metabolic pathway include DsCrtB, DsPDS, DsZ-ISO, DsZDS, DsCRTISO, DsLUT5, DsCrtL-B, and DsCCD8, while the predicted down-regulated genes include DsCrtF, and DsLUT1. The four genes that were both up-regulated and down-regulated were DsZEP, DsCrtR-b, DsCruA/P and DsCrtZ 4. The research results can provide scientific basis for the industrialization practice of D. salina.

Ultrasound assisted techniques for starch modification to develop novel drug delivery systems: A comprehensive study

Starch derived from plants plays an essential role in pharmaceuticals due to its components Amylose and Amylopectin, which form essential granules for drug delivery. Its biocompatibility and cost-effectiveness make it indispensable in pharmaceutical formulations, facilitating controlled drug release and tablet breakdown. The effectiveness and safety of drug formulations are often hindered by challenges such as low solubility and stability. In order to overcome these obstacles, current research is focused on modifying the properties of starch. The goal is to improve its solubility, swelling, erosion, stability, and ability to release drugs. A promising solution that has emerged is ultrasound-based modification. This technique has shown great potential in transforming starch granules, leading to improved solubility, degradability, and control over drug release. Not only is this method efficient and quick, but it also has the added benefit of being eco-friendly. This discussion will explore the mechanisms behind the modification of starch based on ultrasound, delving into both the physical and chemical changes that occur in starch granules. The analysis explores the utilization of modified starch induced by ultrasound in the field of drug delivery, investigating its stability and compatibility with biological systems. By exploring the capabilities and difficulties associated with the use of ultrasound to change starch for the delivery of drugs, we highlighted its potential as a leading and effective methodology.

The Influence of PVP Polymer Topology on the Liquid Crystalline Order of Itraconazole in Binary Systems.

This study presents a novel approach by utilizing poly(vinylpyrrolidone)s (PVPs) with various topologies as potential matrices for the liquid crystalline (LC) active pharmaceutical ingredient itraconazole (ITZ). We examined amorphous solid dispersions (ASDs) composed of ITZ and (i) self-synthesized linear PVP, (ii) self-synthesized star-shaped PVP, and (iii) commercial linear PVP K30. Differential scanning calorimetry, X-ray diffraction, and broad-band dielectric spectroscopy were employed to get a comprehensive insight into the thermal and structural properties, as well as global and local molecular dynamics of ITZ-PVP systems. The primary objective was to assess the influence of PVPs' topology and the composition of ASD on the LC ordering, changes in the temperature of transitions between mesophases, the rate of their restoration, and finally the solubility of ITZ in the prepared ASDs. Our research clearly showed that regardless of the PVP type, both LC transitions, from smectic (Sm) to nematic (N) and from N to isotropic (I) phases, are effectively suppressed. Moreover, a significant difference in the miscibility of different PVPs with the investigated API was found. This phenomenon also affected the solubility of API, which was the greatest, up to 100 μg/mL in the case of starPVP 85:15 w/w mixture in comparison to neat crystalline API (5 μg/mL). Obtained data emphasize the crucial role of the polymer's topology in designing new pharmaceutical formulations.

A rapid and highly sensitive HILIC-HPLC based analytical assay method for quantification of azacitidine and venetoclax in a single run

Venetoclax and Azacitidine combination has recently been approved by the USFDA to treat old people with acute myeloid leukemia. Pharmaceutical formulations of the combination of these two drugs are expected to be launched soon. Till date, an analytical method of any type has not been reported in literature for quantification of Venetoclax and Azacitidine in a single run. The current work set out to establish an HILIC-HPLC based analytical assay method for simultaneous quantification of Azacitidine and Venetoclax from the mixed sample. The method has been developed employing Poroshell HILIC column. Ammonium formate (10 mM, pH 5.0) and acetonitrile were used as a mobile phase in gradient programme. A variety of parameters, including linearity, accuracy, precision, specificity, robustness, and ruggedness were evaluated to validate the method. Azacitidine and Venetoclax were eluted at 8.8 min and 4.0 min, respectively. Method was linear over the range of 1-100 µg/mL. Recovery was found to be 98.29-99.28% and 101.84-101.95% for Azacitidine and Venetoclax, respectively. The method was reproducible with a relative standard deviation of less than two in precision studies. The developed method can suitably be employed for quantifying Venetoclax and Azacitidine in a single run from their mixed samples.

Formation and Application of Starch–Polyphenol Complexes: Influencing Factors and Rapid Screening Based on Chemometrics

Understanding the nuanced interplay between plant polyphenols and starch could have significant implications. For example, it could lead to the development of tailor-made starches for specific applications, from bakinag and brewing to pharmaceuticals and bioplastics. In addition, this knowledge could contribute to the formulation of functional foods with lower glycemic indexes or improved nutrient delivery. Variations in the complexes can be attributed to differences in molecular weight, structure, and even the content of the polyphenols. In addition, the unique structural characteristics of starches, such as amylose/amylopectin ratio and crystalline density, also contribute to the observed effects. Processing conditions and methods will always alter the formation of complexes. As the type of starch/polyphenol can have a significant impact on the formation of the complex, the selection of suitable botanical sources of starch/polyphenols has become a focus. Spectroscopy coupled with chemometrics is a convenient and accurate method for rapidly identifying starches/polyphenols and screening for the desired botanical source. Understanding these relationships is crucial for optimizing starch-based systems in various applications, from food technology to pharmaceutical formulations.

STABILITY BASED HPLC METHOD FOR CYCLOPHOSPHAMIDE RELATED SUBSTANCES IN FINISHED DRUG PRODUCTS: DEVELOPMENT AND VALIDATION

Objective: The current study aimed to develop a simple, sensitive, and precise high-performance liquid chromatographic (HPLC) method for estimating cyclophosphamide and its related substances, as well as to implement the developed method in a capsule product. Methods: Method development was performed using various solvent and buffer-solvent ratios at different flow rates for better resolution and to decrease the run time. The developed method was validated in accordance with the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines. The developed method was implemented to estimate the amount of cyclophosphamide and its related substances. Results: Chromatographical conditions were optimised, and the best chromatographical conditions with adequate resolution for cyclophosphamide and its related substances were achieved using the enable X-Bridge C18 column, using a mobile phase combination of phosphate buffer pH 7.0, water, methanol, and acetonitrile at a flow rate of 0.5 ml/min. The detection was monitored at a wavelength of 200 nm. The developed method was validated for system suitability, specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, precision, accuracy and robustness. The results indicate that the method was sensitive and could detect and quantify lower levels of cyclophosphamide and its related substances. The linearity range was from LOQ to 150 %, and a correlation coefficient ranging from 0.9987 to 0.9999 indicates that at this concentration range, substances were highly linear. This was further supported by satisfactory forced degradation studies. Conclusion: The developed analytical method is simple, precise, and reproducible and thus can be used for the stability-indicating analysis of cyclophosphamide and its related substances in pharmaceutical formulations.

Development and Validation of a RP-HPLC Method for the Simultaneous Determination of Silver Sulfadiazine and Sodium Hyaluronate in the Presence of Methyl and Propyl Paraben in a Pharmaceutical Cream for Burns.

A direct and precise isocratic RP-HPLC method for simultaneous determination of silver sulfadiazine (SSD) and sodium hyaluronate (SH) in the presence of methyl (MP) and propyl parabens (PP) was developed and validated. Agilent chromatograph with X-Select C18 column (250 × 4.6mm2, 5μm) was used. Chromatographic separation was achieved using a mobile phase consisting of acetonitrile and 0.05M phosphate buffer (pH5.0 to which added triethyl amine 0.5ml/L), at a ratio 35: 65v/v. Elution was used at flow rate of 1.0mL/min at ambient temperature with UV detection at 205nm. The retention times for SH, SSD, MP and PP were 1.49, 3.3, 6.7 and 19.5min, respectively. The presented chromatographic method was fully validated in accordance with ICH requirements, it was valid over linearity ranges of (0.80-100.00μg/mL) and (3.20-100.00μg/mL) for SSD and SH, respectively. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges and the sensitivity of the method, as the limits of detection and quantification for each active ingredient was also determined. The validated method was successfully applied for the quantification of SSD and SH in pharmaceutical cream formulation and the mean recovery %±SD were 100.93 ± 0.985 and 100.05 ± 0.668 for SSD and SH; respectively, indicating satisfactory accuracy of the method.

Utility of Localized Surface Plasmon Resonance of Gold Nanoparticles for Spectrophotometric Determination of Dobutamine in Pharmaceutical Formulations

Utility of Localized Surface Plasmon Resonance of Gold Nanoparticles for Spectrophotometric Determination of Dobutamine in Pharmaceutical Formulations

Sensitive and validated UPLC-MS/MS method for the identification and characterization of forced degradation products for felodipine

AbstractA rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.

From Scraps to Solutions: Harnessing the Potential of Vegetable and Fruit Waste in Pharmaceutical Formulations

Background:: Food waste is a major worldwide problem due to the increasing population and imbalances in supply chains. Waste from fruits and vegetables are a substantial proportion of the overall food waste generated, accounting for approximately 42% of the waste produced. Methane, a strong greenhouse gas with a significant potential for global warming, is produced when these waste products are typically dumped in landfills. Objectives:: The study's goal is to present a thorough overview of the most recent findings and developments in the use of vegetable and fruit waste for creating therapeutic formulations. Recognizing the opportunities and challenges in this developing area of study, as well as the promise that vegetable and fruit waste contains for the creation of environmentally friendly and economically advantageous pharmaceutical formulations. Methods:: A comprehensive review of existing literature on the utilization of vegetable and fruit waste in pharmaceutical formulations was conducted. The review included studies on the chemical composition and bioactive compounds present in various types of vegetable and fruit waste, their extraction methods, and their potential applications in pharmaceutical formulations. Additionally, current waste management practices and challenges associated with waste disposal were also analyzed. Conclusion:: The review highlights the significant potential of vegetable and fruit waste in the development of pharmaceutical formulations. Fruit and vegetable waste offer a wide range of bioactive compounds, such as antioxidants, antimicrobials, and antiinflammatory agents, which could be utilized in drug formulation. Moreover, this approach can promote environmental sustainability by reducing waste generation and enhancing waste utilization. Further research and development efforts should focus on optimizing extraction methods, evaluating the efficacy and safety of wastederived compounds, and addressing regulatory requirements for integrating vegetable and fruit waste into pharmaceutical products. Harnessing the potential of vegetable and fruit waste in pharmaceutical formulations can lead to sustainable advancements in the pharmaceutical industry while addressing environmental concerns.

Development and Evaluation of Chemometric Models for the Estimation of Sumatriptan in the Presence of Naproxen and a Degradation Product Using UV Spectrophotometry.

Chemometrics is a discipline that allows the spectral resolution of drugs in a pharmaceutical formulation along with degradation product and it is as an alternative to chromatographic methods. Sumatriptan (SUM) is co-formulated with naproxen (NAP) and used in acute migraine attacks. SUM which has physiological importance has not been subjected to any stability-indicating chemometric approaches yet so there is a need for accurate and safe method for the assay of the cited drug in their preparation. SUM was determined in pharmaceutical formulation along with NAP and in presence of alkali-induced degradation product with simple and cost-effective multivariate approaches using spectrophotometric data. The greenness and blueness assessment was applied using different ecological metrics, including green analytical procedure index (GAPI), analytical greenness metric (AGREE), analytical eco-scale (AES) & new "blueness" evaluation using BAGI tool, respectively. Three chemometric approaches were applied for the stability-indicating determination of SUM in presence of NAP. Classical least squares (CLS), Partial least squares (PLS) and Principal components regression (PCR), three multivariate calibration numerical models that were performed on the UV- spectra of the mixtures, were used to achieve the best resolution. Sumatriptan was analyzed with mean accuracies for PLS (100.29 ± 1.318) and for PCR (100.60 ± 1.564). The presented methods were compared and validated for their quantitative analyses. Moreover, statistical comparison between the results obtained by the proposed models and the official methods showed no significant differences. The proposed multivariate calibrations were accurate and specific for quantitative analysis of the studied component. PLS is the best method that has the capacity for qualitative analysis of SUM and it is suitable for routine analysis and stability studies of it in quality control laboratories. Various ecological assessment metrics confirmed the long-standing eco-friendliness of the suggested models.

Simultaneous sensing of carbidopa and levodopa by a novel strategy based on dual-emission ratiometric assay of modified carbon dots.

Rapid control of the content of Parkinson's drugs in biological fluids and pharmaceutical formulations is of great importance because changes in the concentration of these drugs affect their bioavailability and biopharmaceutical properties. Therefore, we presented a simple and convenient method for the ratiometric detection of carbidopa and levodopa for carbon dots (CDs) dual-fluorescent emission. Dual-emission CDs were prepared from chitosan using a microwave method, following which the surface was chemically modified with terephthalaldehyde. CDs had two strong well-separated peaks at 445 and 510nm. The relative measurement of carbidopa and levodopa was based on the static extinction of CDs at 445nm and increase at 510nm, respectively. The linear range for carbidopa measurement was 2.5-300nM, with a limit of detection (LOD) of 2.1nM, and a relative standard deviation (RSD) of 1.68%. Further, the linear range for levodopa measurement was equal to 3.0-400nM, with LOD and RSD% of 2.8nM and 3.5%, respectively. Also, selectivity of ratiometric sensor in the presence of interferences was investigated, which showed that the recovery of carbidopa and levodopa in serum and urine samples has changed between 96.80% and 116.24% with RSD% 0.11-0.77. CDs also provided good results for the determination of carbidopa and levodopa in real samples, and had high selectivity in the presence of possible interferences.

Impact of Cross‐Linking on the Physicochemical and Physiological Characteristics of Barnyard Millet (Echinochloa frumentacea) Grains Starch

Barnyard millet starch (Echinochloa frumentacea) has been investigated for its potential in drug delivery systems due to its unique properties. This study examined the physicochemical and physiological properties of cross‐linked barnyard millet starch (BMS) using varying concentrations of sodium tripolyphosphate (STPP). Physicochemical and physiological properties of the cross‐linked starches are analyzed. Cross‐linking resulted in reduced swelling capacity and solubility of starch samples. Morphological analysis revealed rough surfaces with cavities and minute cracks in cross‐linked starches. Acute and sub‐acute toxicity studies in test animals indicated no adverse effects, with LD50 values within acceptable limits at 2000 mg kg−1. Hematological, biochemical, and lipid profiles showed no significant alterations compared to the control group. The study demonstrated a low acute toxicity level and favorable safety profile for STPP‐cross‐linked starch. These findings highlighted the potential of cross‐linked barnyard millet starch as a carrier in drug delivery system and for food applications. This study supports the potential of cross‐linked barnyard millet starch in pharmaceutical formulations.