Percentage Purity Research Articles

Identification and in vitro genotoxicity assessment of forced degradation products of glimepiride and glyburide using HEK cell-based COMET assay.

This study focuses on characterizing the forced degradation products of antidiabetic drugs glimepiride (GMD) and glyburide (GBD), with previously unexplored genotoxicity. Drugs underwent stress induced by acid, base, and hydrogen peroxide. For GMD, impurities were profiled and isolated using Hypersil Gold C8 (250 × 10 mm, 5μ) through semi-preparative HPLC with a fraction collector. For GBD, impurity profiling was performed using semi-preparative HPLC (Hypersil GOLD C18, 250 × 10 mm, 5μ), and reverse-phase flash chromatography (FP ECOFLEX C18 4g column) for isolation. Although five GMD and three GBD impurities were detected, only three GMD and two GBD impurities were separated and assessed for purity using analytical RP-HPLC with the purity percentages ranging from 96.6% to 99.9%. LC-Orbitrap MS was used to identify these three GMD impurities (m/z: 408.122, 338.340, 381.160) and two GBD impurities (m/z: 369.065, 325.283). ProTox-II in silico predictions classified all impurities as class 4 and 5, with no positive genotoxicity indications. In vitro comet assays, using HEK cells, indicated that for GMD, impurity 2 and impurity 5 were less genotoxic, whereas impurity 4 exhibited genotoxicity. For GBD, both impurities 1 and 3 were found to be genotoxic, with impurity 3 showing a higher level of genotoxicity than impurity 1.

Chromatographic fingerprinting of epiphytic fungal strains isolated from Withania somnifera and biological evaluation of isolated okaramine H.

Medicinal plants are "goldmines" of natural products, and continue to provide key scaffolds for drug development. They have immense therapeutic potential, encapsulating a plethora of metabolites within them, which have yet to be explored. Withania somnifera (L.) Dunal is one such medicinal plant known since time immemorial for its therapeutic activity in the Ayurveda system of medicine. Studies have revealed Nature's marvel of these medicinal plants harbouring endophytic and epiphytic microorganisms from phyllosphere to rhizosphere. Chromatographic fingerprinting was carried out using HPTLC and HPLC on five epiphytic strains isolated from the leaves, stem and fruits of Withania somnifera. Out of five filamentous fungi, one fungus identified as Aspergillus aculeatus S20 was well explored. An indole alkaloid, okaramine H, was isolated using systematic chromatographic investigation at a retention time of 26.278 min showing λmax at 206, 236, 284 and 370 nm. Confirmation was achieved using NMR and mass spectrometry (MS) as analytical techniques. Structure elucidation was done by studying the fragmentation pattern using MS/MS and an accurate mass was determined using HR-ESI-QTOF-MS showing m/z of 521.2546 [M + H]+. The percentage purity of isolated okaramine H was found to be >90. Well known for its insecticidal activity, okaramine H was explored for its antileishmanial activity against the Leishmania donovani parasite for the first time. Under in vitro conditions, the compound showed an inhibitory effect on Leishmania donovani promastigotes with an IC50 of 147 μg mL-1.

Optimization of thorium solvent extraction process from feed solution with Cyanex 272 by response surface methodology (RSM)

Due to the limited reserves of uranium, the abundance of thorium compared to it and other advantages, the development of the thorium fuel cycle is of interest in different countries. The optimization of thorium extraction from a feed solution produced by Saghand ore with bis(2,4,4-trimethylpentyl) phosphinic acid (Cyanex 272) on a laboratory scale was evaluated by response surface method. The operating variables include Cyanex 272 concentration of 0.001 to 0.2 mol/L, pH of 0 to 2, equilibrium time of 5 to 60 min and aqueous to organic phase ratio of 0.5 to 2.5 were conducted. The value of R2 = 0.9695 and an error of less than 4% indicate the validity of the model. Therefore, the model is in good agreement with the experimental results. It can be said that there are significant interactions between operational parameters, which vindicate different feedbacks of the system in different operational conditions. The results showed that the 4 mol/L sulfuric acid was a suitable agent for recovering thorium ions from the loaded organic phase. In optimum conditions, the thorium purity percentage and thorium stripping efficiency were obtained 98.99 and 94.12%, respectively.

Dendritic cell vaccines as cancer treatment: focus on 13 years of manufacturing and quality control experience in advanced therapy medicinal products

Background aimsDendritic cells (DCs) are professional antigen-presenting cells of the mammalian immune system. Ex vivo differentiated DCs represent a unique Advanced Therapy Medicinal Product (ATMP), used in several clinical trials as personalized cancer immunotherapy. The therapy's reliability depends on its capacity to produce high-quality mature DCs (mDCs) in compliance with Good Manufacturing Practices. AimsFrom March 2010 to December 2023, 103 patients were enrolled in multiple clinical trials at the Immuno-Gene Therapy Factory at IRCCS Istituto Romagnolo per lo Studio dei Tumori (IRST) “Dino Amadori”. Six hundred forty-two doses were produced, and the manufacturing process was implemented to optimize production. Our study is a retrospective analysis focusing on the quality control results. MethodsWe retrospectively analyzed the results of the quality control tests carried out on each produced batch, evaluating viability, purity and phenotype of mDCs and their quality in terms of microbiological safety. The data obtained are given with median and interquartile range. ResultsThe batches were found to be microbiologically safe in terms of sterility, mycoplasma, and endotoxins. An increase in DC maturation markers was found. The release criteria checks showed a high percentage of viability and purity was maintained during the production process. ConclusionsOur findings have confirmed that the measures implemented have ensured the safety of the products and have contributed to the establishing a robust “Pharmaceutical Quality System.” This has enabled many safe mDCs to be produced for clinical trials.

Reduction of Methylene Blue Using Silica Nanoparticles Obtained from Waste ZrC

AbstractThe study conducted an extraction of pure amorphous nano‐silica (SiO2 NP) from waste product at the ZrC factory. Various techniques such as TEM, SEM‐EDX, ICP, XRD, FTIR, BET, and DLS were utilized to synthesize and characterize the silica nanoparticle. The results showed successful production of pure amorphous silica, with no discernible difference in purity percentage between samples prepared with or without acidic pre‐treatment. It was found that the leaching temperature, process time, and reactant ratio all played a role in the production of nano‐silica. The ideal leaching temperature was determined to be 368 K, with an optimal process time of 2 h. The weight ratio of WPZF/NaOH that yielded the highest percentage of silica extraction was 9 : 10. Additionally, at pH 7, the nano‐silica exhibited the best specific surface area (BET) of 472.51 m2/g. The average size of the spherical nano‐silica, as determined by DLS, was approximately 38 nm. Furthermore, the produced nano‐silica was found to be an effective catalyst for the treatment of methylene blue (MB). MB could be degraded by more than 99 % of the initial concertation (10 mg/L) in the presence of NaBH4 within 16 min and rate constant of the catalytic reduction achieved as 0.134 min−1. These findings demonstrate the potential of amorphous nano‐silica as a valuable resource in various applications.

Bioestimulante para maturação de cana-de-açúcar em lavouras fertirrigadas por gotejamento

ABSTRACT In irrigated fields, sugarcane’s vegetative growth and carbohydrate consumption during ripening require ripener management options to improve crop yield. The hypothesis is that ripeners, together with nutrients, biostimulants, and amino acids, improve physiological responses that favor the quality of the raw material and increase the sucrose content. Consequently, the study aimed to evaluate the agro-industrial response of a fertigated sugarcane crop to ripening agents. The treatments consisted of applying chemical ripener (CR), nutritional ripener (NR), and a joint application of NR+CR, besides control with four replicates. Agro-industrial attributes (total soluble solids, apparent sucrose (AS), reducing sugars (RS), total recoverable sugar (TRS), purity, fiber, sucrose in the stalk (SS) were evaluated at 0 (before application), 12, 19, 36, and 60 days after application (DAA). The time modified the technological attributes of sugarcane under ripener application. The highest apparent sucrose and total soluble solids values were obtained with NR+CR compared to the control. The NR and NR+CR treatments presented the highest TRS contents (150 kg Mg-1) at 36 DAA. Furthermore, the NR+CR treatment increased fiber content but did not compromise the quality of the raw material, and it showed high contents of SS and purity percentage, as well as low contents of RS. The chemical and nutritional ripeners efficiently promoted sugarcane ripening in areas without drying off before harvest. NR application at the end of the cycle can potentially increase sugar yield.

UV spectrophotometric determination of chlorthalidone in tablet dosage form by using single point standardization method

The current research endeavors to elucidate the creation of an uncomplicated, highly sensitive, swift, precise, and cost-effective UV-accepted spectrophotometric method for the quantitative assessment of Chlorthalidone. This is achieved through the utilization of a visible spectrophotometric approach employing single-point standardization and calibration plot methods, for pharmaceutical dosage forms. The equipment employed includes a double-beam UV-visible spectrophotometer, specifically the Shimadzu Model UV1800, with 1cm quartz cells and 0.2 M Sodium hydroxide serving as the solvent. Notably, an absorption maximum is identified at 219 nm. The developed method strictly adheres to Beer’s law. In the case of single-point standardization, the percentage of Chlorthalidone detected falls below the labeled claimed limit. Simultaneously, the tablet formulation is subjected to a percentage purity test using the calibration plot method, revealing that the observed quantity of Chlorthalidone is below the labeled content. This suggests a potential discrepancy in the marketed product of Chlorthalidone, indicating a probable deficiency in the therapeutic effect of the formulation due to the lower amount of Chlorthalidone present. The overall efficacy of the product hinges on the quality assurance of its constituents.

An Eco-Friendly RP-HPLC Method Development and Validation for Quantification of Favipiravir in Bulk and Tablet Dosage Form Followed by Forced Degradation Study.

In this work, an eco-friendly simple, precise reverse phase high-performance liquid chromatography (HPLC) method has been developed and validated for Favipiravir in bulk and tablet dosage form followed by its force degradation study. The proposed method was validated to obtain official requirements including stability, accuracy, precision, linearity, robustness and selectivity as per International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) Guidelines. The estimation was developed on C (18) column reversed-phase using the mobile phase composition as methanol:water (10:90v/v). The flow rate was set as 1ml/min, and the maximum absorption was observed at 323nm using Shimadzu Photo Diode Array detector. The Favipiravir, drug showed a precise and good linearity at the concentration ranges of 10-50μg/mL. The Revearse Phase High Perforance Liquid Chromatography assay showed the highest purity ranging from 99.90 to 100.02% for Favipiravir, tablet dosage form, and 100.15% was the mean percentage purity. The percent recovery was found within the acceptance limit of (98.6-100.0%). Intra- and inter-day precision studies of the method were less than the maximum allowable limit percentage of relative standard deviation ≤ 2.0. The Favipiravir retention time was found to be 5.00min. To examine the stability of the drug, various forced degradation studies were conducted on Favipiravir Active Pharmaceutical Ingredient. The developed method was validated according to the ICH guidelines. A very quick, cost-effective, precise and accurate HPLC method for the determination of Favipiravir has been developed and validated in compliance with ICH guidance Q2.

Combatting Sugar Beet Root Rot: Streptomyces Strains' Efficacy against Fusarium oxysporum.

Sugar beet root rot disease triggered by Fusarium oxysporum f. sp. radicis-betae is a destructive disease and dramatically affects the production and quality of the sugar beet industry. Employing beneficial microorganisms as a biocontrol strategy represents an eco-friendly and sustainable approach to combat various plant diseases. The distinct aspect of this study was to assess the antifungal and plant growth-promoting capabilities of recently isolated Streptomyces to treat sugar beet plants against infection with the phytopathogen F. oxysporum. Thirty-seven actinobacterial isolates were recovered from the rhizosphere of healthy sugar beet plants and screened for their potential to antagonize F. oxysporum in vitro. Two isolates SB3-15 and SB2-23 that displayed higher antagonistic effects were morphologically and molecularly identified as Streptomyces spp. Seed treatment with the fermentation broth of the selected Streptomyces strains SB3-15 and SB2-23 significantly reduced disease severity compared to the infected control in a greenhouse experiment. Streptomyces SB2-23 exhibited the highest protective activity with high efficacy ranging from 91.06 to 94.77% compared to chemical fungicide (86.44 to 92.36%). Furthermore, strain SB2-23 significantly increased plant weight, root weight, root length, and diameter. Likewise, it improves sucrose percentage and juice purity. As a consequence, the strain SB2-23's intriguing biocontrol capability and sugar beet root growth stimulation present promising prospects for its utilization in both plant protection and enhancement strategies.

ASSESSMENT OF YIELD LOSSES CAUSED BY BORER PESTS OF SUGARCANE UNDER CHANGING CLIMATE SCENARIO

The field experiment was conducted during 2021-22 at Central Sugarcane Research Station, Padegaon Maharashtra to assess actual yield loss due to different species of borer pests of sugarcane in changing climatic scenario. There were two treatments, each 0.1 ha size plot for treated and untreated separated by keeping 100 meter distance. Treated plot applied with recommended effective chemical insecticide by soil application of Chlorantroniliprol 0.4 GR @ 18.75 kg/ha and foliar application of Chlorantroniliprol 18.5 % SC @ 375 g/ha following pair plot technique design. Percent infestation of early shoot borer was noticed at 30 DAP, 60 DAP, 90 DAP and 120 DAP in treated plot with recommended effective chemical insecticide were 2.59, 4.22, 6.93 and 0.83, respectively, while in untreated plot were 5.63, 8.06, 10.08 and 2.78, respectively. The cumulative percentage incidence of early shoot borer was found in 3.637 % in treated plot and 6.817 % in untreated plot. Total number of bored plants / ha was 3637 in treated plot and 6817 in the untreated plot. Whereas, per cent incidence of Internode borer in treated plot with recommended effective chemical insecticide and untreated plot showed a 1.50% and 4.40% in untreated plot, respectively. Top borer was not observed throughout the crop period in both plots. Among different treatments, plot treated with recommended effective chemical insecticide recorded highest germination percent (60.40 %), No. of milliable cane (87.50 thousands ha-1), Average cane weight (1.265 kg) and Yield (101.25 t/ha) in treated plot as against untreated plot. The brix percentage, purity percentage, sucrose content and CCS% in treated with recommended effective chemical insecticide were recorded as 23.37, 92.28, 20.96 and 14.22, respectively, while in untreated plot were recorded as 22.68, 89.68, 20.93 and 14.12, respectively

Synthesis of calcium propionate from indigenous limestone from Swat area in Pakistan

In this study, native limestone from the Swat area of Pakistan was used for the synthesis of calcium propionate. The powdered limestone was allowed to react with propionic acid and the effect of the synthesis parameters, that is, the particle size (50, 100, 150, and 200 mesh), propionic acid (10, 15, and 30 %), solid-liquid ratio (0.1:10, 0.12:1, 0.14:1, and 0.16:1), reaction time (1, 1.5, 2, and 2.5 hours) and the temperature (60, 80, 90, and 100 °C) on the percentage yield and purity of calcium propionate was studied. The results showed that the optimum synthesis parameters were 200 mesh particle size, 15% propionic acid concentration, 0.14:1 solid-liquid ratio, 2.5 hours reaction time, and 80 °C temperature. The product obtained under optimal conditions was characterized by infrared spectroscopy, thermogravimetry, and scanning electron microscopy. The results revealed that a product having ≥ 99.8% purity with 85% yield can be obtained by this process.

Analytical Methods of Estimation of Oxetacaine and its quality determinations in different Pharmaceutical Formulations by Reverse Phase High Performance Liquid Chromatography (RP-HPLC)

Objective: The aim of the current research was to design and develop an analytical method for the estimation of Oxetacaine and its quality control determinations of different formulation by reverse phase high performance liquid chromatography (RP-HPLC). Method: In Method I the Agilent HPLC used for the Estimation purpose. C-18 column (250 X 4.6mm i.e., 1µ) as stationary phase and 0.05% formic acid buffer: Methanol in the ratio 30:70 % v/v as mobile phase, with a flow rate of 1.0ml/min. Diluents of Methanol: water 90:10 ratio used for the study with ambient Temp conditions. In Method II the Agilent HPLC used for the Estimation purpose .C8 Column ((250 X 4.6mm i.e., 5µ) as stationary phase and ammonium phosphate buffer pH 4.8: Acetonitrile in the ratio 25:75 % v/v as mobile phase, with a flow rate of 0.9ml/min. Diluents of Acetonitryl: water 50:50 ratios used for the study with ambient Temp conditions. Result: Method 1: Oxetacaine standard (86µg/ml concentration) peak was eluted at average of 5.629min at 3 runs with Asymmetry of 1.29813 and Peak area of 23237896 with the conditions of %RSD of max2. With qualifying of system suitability, accuracy and reproducibility. Some of Marketed suspension formulations were operated under the same instrument conditions and the results were compared with standard Oxetacaine to ensure the percentage purity of Marketed suspensions. Method 2: Oxetacaine standard (196µg/ml concentration) peak was eluted at average of 4.884 min at 3 runs with Asymmetryof1.17244 and Peak area of 360543170 with the conditions of %RSD of max 2. With qualifying of system suitability, accuracy and reproducibility. Some of Marketed suspension formulations were operated under the same instrument conditions and the results were compared with standard Oxetacaine to ensure the percentage purity of Marketed suspensions. Conclusion: The two new method of estimation of oxetacaine like using Method 1: C18 column, 0.05% formic acid buffer: Methanol in the ratio 30:70 % v/v as mobile phase @214nm and Method 2: C8 Column, ammonium phosphate buffer pH 4.8: Acetonitrile in the ratio 25:75 % v/v as mobile phase @214 achieved with simple, precise, accurate and sensitive. In addition the quality control estimating of some of random of F1, F2, F3, F4, F5, and F6 marketed oxetacaine suspensions were analysed using this Two Optimized methods. Out of 6 formulations, 2 formulations F3, F6 determined as substandard quality on the both the methods. Hence proving these two new methods optimal for the further monograph inclusions as well as quality control predictions of oxetacaine in API as well as Finished Pharmaceutical Formulations.

COMPARISON OF CALCIUM OXALATE CONCENTRATIONS WITH DIFFERENT EXTRACTION METHODS IN PORANG FLOUR (AMOPHALUS MUELLERI BLUME)

This study aims to compare the concentration of calcium oxalate in porang flour (Amophalus Muelleri Blume) using different extraction methods. The extraction method used is direct (non-stratified) extraction and stratified extraction. The percentage of purity of porang flour from multistage and non-stratified extraction, respectively, was 2.16% and 2.62%. Efficiency of ethanol content in the direct/non-staged purification process is 80% ethanol, while for the graded efficiency the levels are 40%, 60%, and 80%. Visual observations including flour color, viscosity, and proximate test showed purification of porang flour using graded extraction gave better results than ordinary/unstaged extraction.

Microbial bioethanol production from locally sourced corncobs through saccharification and fermentation using Aspergillus niger and Saccharomyces cerevisiae


 The utilization of agricultural residues, specifically corncobs, as a renewable feedstock for bioethanol production holds promise in sustainable energy generation. This study investigates the feasibility of microbial bioethanol production from locally sourced corncobs through co-digestion involving Aspergillus niger and Saccharomyces cerevisiae. The process involved washing the corncobs, grinding them, and then hydrolyzing the corncob flour with cultured Aspergillus niger. The resulting sugar syrup was then fermented with Saccharomyces cerevisiae to produce ethanol. The process was optimized to obtain the highest ethanol yield. The results indicated that the process developed achieved a maximum ethanol yield of 33.2, 36.7, and 45.5% from the triplicate digesters used with a percentage purity in the range of 62.06% to 87.69% and a mean volume of ethanol recovery of 145 mL per 400 mL of the fermented product. This yield was obtained when the temperature of the hydrolysis using inoculum and saccharification were maintained at 27 °C. Additionally, the optimal substrate concentration for maximum ethanol yield was found to be 50 % (w/v). The study demonstrates the potential of corncobs obtained from local mashing as a source of fermentable sugars for the microbial production of bioethanol. Additionally, the results provide a basis for the development of an efficient and economically feasible process for production of bioethanol from corncobs obtained from local mashing.

Detection of True Hybrids in Pearl Millet Cross Combinations by Employing SSR Molecular Markers

Pearl millet (Pennisetum glaucum L. R. Br.), a crucial staple food and significant cereal crop, is gaining prominence due to its versatile applications as feed, food, and fodder. Heterosis of this crop has been extensively harnessed to increase productivity. Hybrid variants exhibit superior grain and stover yields compared to open-pollinated varieties.Top of Form The primary aim of this investigation was to evaluate and confirm authentic hybrids within three resultant F1 progenies. The assessment of parents and F1 hybrids was carried out during the Kharif 2021for the purpose of accurate discrimination and rapid verification of true hybrids by employing 20 SSR molecular markers. The experimental materials consisted of three distinct cytoplasmic male sterile (CMS) lines including ICMA 843-22, ICMA 04999, and ICMA 02333, used as female parents along with three fertility restorers, viz., ICMR 01004, ICMR 20233, and ICMR 20342, were utilized as male parents. The analysis of SSR profiles was based on distinctive banding patterns, resulting in unique profiles for the hybrids. The amplified fragment sizes ranged between 90 to 300 base pairs (bp), effectively enabling the differentiation of authentic hybrids. Within the specific crosses, the percentage of polymorphism was determined 75% for the cross ICMA 843-22 × ICMR 01004, 80% for the cross combination ICMA 04999 × ICMR 20233, and 75% for the cross ICMA 02333 × ICMR 20342. The true hybrids were calculated using hybrid purity percentage formula using heterozygous banding patten among total plants evaluated. Among a total of 100 F1 plants, 85, 86, and 88 plants were accurately identified as true hybrids in the respective crosses i.e., ICMA 843-22 × ICMR 01004, ICMA 04999 × ICMR 20233, and ICMA 02333 × ICMR 20342. The identified markers hold significant potential for applications such as hybridity test, genetic purity assessments, diverse germplasm identification, and DNA fingerprinting endeavors in future.

EXTRACTION, IDENTIFICATION AND ESTIMATION OF CAFFEINE IN GREEN AND BLACK TEA SAMPLES BY A SIMPLE UV-VISIBLE SPECTROSCOPIC METHOD

Caffeine is a widely consumed psychoactive compound present in coffee, tea, soft drinks, energy drinks, and chocolates. It is a diuretic and a central nervous system (CNS) stimulant. Apart from stimulating the CNS, it exerts beneficial effects in combination with other substances like L-theanine and catechins. Caffeine was extracted from green tea and black tea samples using various solvents. The maximum yield of caffeine was obtained from dichloromethane extracts. The extracted caffeine was identified by TLC and FTIR. A simple UV spectroscopic method was developed and validated for the estimation of caffeine in green tea and black tea. The wavelength maximum of caffeine was obtained at 272 nm in distilled water. The Beer-Lambert law was obeyed in the concentration range of 0.5 to 35 µg mL-1 for caffeine. The linearity, accuracy, precision, robustness, and ruggedness, limit of detection and limit of quantification of this method are within the limits of ICH guidelines. This method was found to be precise as % RSD was less than two. The LOD and LOQ values were 0.03 µg mL-1 and 0.091 µg mL-1,respectively. The percentage purity of caffeine from green tea and black tea samples was found to be 98.32% and 99.42 %. Thus, the proposed method was found to be rapid, specific, precise and accurate for the routine analysis of caffeine in green and black tea samples.

The Comparison of Hydrogen Purity on Brown’s Gas Using Dry Cell Electrolyzer with/without Polyvinyl Alcohol (PVA) Separator Membrane

Global environmental issues that demand good air quality have encouraged various energy sources to develop environmentally friendly energy. Brown’s Gas is produced by using an electrolysis system to separate water into Hydrogen (H2) and Oxygen (O2) gas. The dry cell is an electrolyzer that is widely used for both small and large-scale hydrogen production systems. A dry cell electrolyzer was designed with 12 stages of 316 stainless steel with Polyvinyl Alcohol as a polymer membrane to prevent mixing H2 and O2 to get a high percentage of hydrogen purity. This study compares hydrogen purity on Brown’s gas using a dry cell electrolyzer with PVA with/without a PVA separator membrane. The result shows that the PVA membrane significantly impacted hydrogen purity. The hydrogen purity on Brown’s gas without PVA membrane for KOH, NaOH, KCl, and Seawater was 58.37%, 56.42 %, 50.16%, and 55.22 %. Compared to using the membrane was 78.32%, 77.80%, 63.16%, and 74.0 %, with the highest hydrogen obtained was KOH electrolyte.

Investigation into Brazilian Palygorskite for Its Potential Use as Pharmaceutical Excipient: Perspectives and Applications.

Palygorskite is an aluminum and magnesium silicate characterized by its fibrous morphology, providing it with great versatility in industrial applications, including pharmaceuticals. Although most of the reserves are in the United States, in recent years occurrences of commercially exploited deposits in Brazil have been recorded, mainly in the country's northeast region. This has motivated this study, which analyzes raw Brazilian palygorskite compared to a commercial sample (Pharmasorb® colloidal) to demonstrate its pharmaceutical potential. The chemical and mineral composition of the samples were evaluated for surface properties, granulometry, morphology, crystallography, thermal analysis, and spectroscopy. Raw palygorskite presented 67% purity, against 74% for Pharmasorb® colloidal. The percentage purity relates to the presence of contaminants, mainly carbonates and quartz (harmless under conventional conditions of pharmaceutical use). Furthermore, it was possible to confirm the chemical composition of these phyllosilicates, formed primarily of silicon, aluminum, and magnesium oxides. The crystallographic and spectroscopic profiles were consistent in both samples, showing characteristic peaks for palygorskite (2θ = 8.3°) and bands attributed to fibrous phyllosilicates below 1200 cm-1, respectively. The thermal analysis allowed the identification of the main events of palygorskite, with slight differences between the evaluated samples: loss of water adsorbed onto the surface (~85 °C), removal of water contained in the channels (~200 °C), coordinated water loss (~475 °C), and, finally, the dehydroxylation (>620 °C). The physicochemical characteristics of raw palygorskite align with pharmacopeial specifications, exhibiting a high specific surface area (122 m2/g), moderately negative charge (-13.1 mV), and compliance with the required limits for heavy metals and arsenic. These favorable technical attributes indicate promising prospects for its use as a pharmaceutical ingredient in the production of medicines and cosmetics.

SPECTROPHOTOMETRIC FINGERPRINTING AND CHEMICAL DETERMINATION OF STREPTOMYCIN, AMIKACIN, NEOMYCIN, AND GENTAMYCIN SULPHATE BY CONDENSING WITH NINHYDRIN REAGENT

Objective: The study aimed to develop a simple, efficient, inexpensive, rapid, and reproducible spectrophotometric analytical technique for aminoglycosides analysis by condensing with ninhydrin reagent. Methods: At a pH of 8.0, different aminoglycosides, including amikacin, gentamycin, neomycin, and streptomycin, were deaminated by the ninhydrin reagent. The working standard solution for each component was accurately placed into a series of 10 ml calibrated volumetric flasks, then 1 ml of the ninhydrin reagent was added and heated in a water bath for 15 min. The wavelength(s) of maximum absorption(s) was recorded after scanning the resultant purple complex from 350 nm to 930 nm. The final working concentrations ranged between 1600 and 2000 ug/ml. Results: The average weight of a neomycin sulphate tablet was 0.747g, with a standard deviation of 0.667%. After complexing with ninhydrin reagent at pH 6.0 for 10 to 15 min, all aminoglycosides developed purple coloration that lasted beyond 24 h, compared to the initial white, pale yellow, and colorless appearance of streptomycin, amikacin, neomycin, and gentamycin, respectively. The scanned spectra of the purple complex of ninhydrin formed after reaction with aminoglycosides in the visible region (350-900 nm) were similar, indicating the presence of a common parent structural moiety. At 550 nm, 650 nm, 750 nm, and 850 nm, distinct absorptions were observed. Amikacin, Streptomycin, and Gentamicin had the highest absorbance between 800 and 900 nm. After the reaction with ninhydrin, three distinct absorbances were observed in the Neomycin spectrum: between 380 and 400 nm, 580 and 600 nm, and around 800 nm. The comparative spectra for the four aminoglycosides and ninhydrin reagent with blank show a unique feature for the compounds. The coefficients of regression were 0.996 and 0.995, respectively. Conclusion: The proposed methods for analyzing streptomycin in streptomycin injections were successful. The percentage purity ranged from 017–110 % at 650 and 850 nm, which corresponds to the British Pharmacopoeia (BP) limit that streptomycin sulphate tablets should be between 97.00 and 110%.

UV Spectrophotometric and UPLC assay methods for the determination of Palbociclib in bulk and Tablet Dosage Form

The goal of this study was to create a sensitive and reliable UV-spectrophotometric and reverse phase liquid chromatographic method for determining Palbociclib in bulk and pharmaceutical dosage forms. The current UV approach uses methanol and phosphate buffer as a solvent to evaluate absorption at a maximum wavelength of 220nm. Waters Acquity BEH C18 (2.1 x 50mm, 1.7µm) UPLC column with Empower 2 was used in the UPLC procedure. The mobile phase was made up of 50:50 (v/v) methanol and phosphate buffer.The drug obeyed Beer Lambert's law in the UV technique in the concentration range of 1-70µg/ml with a regression coefficient of 0.999. The linearity level in the UPLC technique was 1-100µg/ml. In the validation investigation, the developed UV and UPLC procedures were successful. For the UPLC and UV methods, the percentage purity of the marketed dosage form of Palbociclib was found to be 98.76 percent and 98.84 percent, respectively. The percent RSD of all validation parameters investigated, as suggested by the ICH recommendations, was determined to be less than 2 in both techniques. The two methods established for determining Palbociclib in bulk and tablet doses were found to be accurate, simple, and validated.