Search results for: drug kinetics

Authors: Manisha Choudhary, Sudarsan Neogi

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Malachite green (MG), an organic basic dye, has been widely used for the dyeing purpose, as well as a fungicide and antiseptic in aquaculture industry to control fish parasites and disease. However, MG has now turned out to be an extremely controversial compound due to its adverse impact on living beings. Due to high toxicity, proper treatment of wastewater containing MG is utmost important. Among different available technologies, adsorption process is one of the most efficient and cost-effective treatment method due to its simplicity of design, ease of operation and regeneration of used materials. Nonetheless, commercial activated carbon is expensive leading the researchers to focus on utilizing natural resources. In the present work, a species of cactus, Opuntia ficus-indica (OFI), was used to develop a highly efficient, low-cost powdered activated carbon by chemical activation using NaOH. The biosorbent was characterized by Fourier-transform infrared spectroscopy, field emission scanning electron microscope, energy-dispersive X-ray spectroscopy, Brunauer–Emmett–Teller (BET) and X-ray diffraction analysis. Batch adsorption studies were performed to remove MG from an aqueous solution as a function of contact time, initial solution pH, initial dye concentration, biosorbent dosages, the presence of salt and temperature. By increasing the initial dye concentration from 100 to 500 mg/l, adsorption capacity increased from 165.45 to 831.58 mg/g. The adsorption kinetics followed the pseudo-second-order model and the chemisorption mechanisms were revealed. The electrostatic attractions and chemical interactions were observed between amino and hydroxyl groups of the biosorbent and amine groups of the dye. The adsorption was solely controlled by film diffusion. Different isotherm models were used to fit the adsorption data. The excellent recovery of adsorption efficiency after the regeneration of biosorbent indicated the high potential of this adsorbent to remove MG from aqueous solution and an excellent cost-effective biosorbent for wide application in wastewater treatment.

Keywords: adsorption, biosorbent, cactus, malachite green

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Authors: Oktavia Eka Puspita

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The possibility of using Solid Lipid Nanoparticles (SLN) for topical use is an interesting feature concerning this system has occlusive properties on the skin surface therefore enhance the penetration of drugs through the stratum corneum by increased hydration. This advantage can be used to enhance the drug penetration of topical delivery such as Diclofenac sodium for the relief of signs and symptoms of osteoarthritis, rheumatoid arthritis and ankylosing spondylitis. The purpose of this study was focused on the preparation and physical characterization of Diclofenac sodium loaded SLN (D-SLN). D loaded SLN were prepared by hot homogenization followed by ultrasonication technique. Since the occlusion factor of SLN is related to its particle size the formulation of D-SLN in present study two formulations different in its surfactant contents were prepared to investigate the difference of the particle size resulted. Surfactants selected for preparation of formulation A (FA) were lecithin soya and Tween 80 whereas formulation B (FB) were lecithin soya, Tween 80, and Sodium Lauryl Sulphate. D-SLN were characterized for particle size and distribution, polydispersity index (PI), zeta potential using Beckman-Coulter Delsa™ Nano. Overall, the particle size obtained from FA was larger than FB. FA has 90% of the particles were above 1000 nm, while FB has 90% were below 100 nm.

Keywords: solid lipid nanoparticles, hot homogenization technique, particle size analysis, topical administration

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Authors: Raimoana Frogier, Luc Girard, Pierre Bauduin, Diane Rebiscoul, Olivier Diat

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Nano-ions (NIs) are ionic species or clusters of nanometric size. Their low charge density and the delocalization of their charges give special properties to some of NIs belonging to chemical classes of polyoxometalates (POMs) or boron clusters. They have the particularity of interacting non-covalently with neutral hydrated surface or interfaces such as assemblies of surface-active molecules (micelles, vesicles, lyotropic liquid crystals), foam bubbles or emulsion droplets. This makes possible to classify those NIs in the Hofmeister series as superchaotropic ions. The mechanism of adsorption is complex, linked to the simultaneous dehydration of the ion and the molecule or supramolecular assembly with which it can interact, all with an enthalpic gain on the free energy of the system. This interaction process is reversible and is sufficiently pronounced to induce changes in molecular and supramolecular shape or conformation, phase transitions in the liquid phase, all at sub-millimolar ionic concentrations. This new property of some NIs opens up new possibilities for applications in fields as varied as biochemistry for solubilization, recovery of metals of interest by foams in the form of NIs... In order to better understand the physico-chemical mechanisms at the origin of this interaction, we use silicon wafers functionalized by non-ionic oligomers (polyethylene glycol chains or PEG) to study in situ by X-ray reflectivity this interaction of NIs with the grafted chains. This study carried out at ESRF (European Synchrotron Radiation Facility) and has shown that the adsorption of the NIs, such as POMs, has a very fast kinetics. Moreover the distribution of the NIs in the grafted PEG chain layer was quantify. These results are very encouraging and confirm what has been observed on soft interfaces such as micelles or foams. The possibility to play on the density, length and chemical nature of the grafted chains makes this system an ideal tool to provide kinetic and thermodynamic information to decipher the complex mechanisms at the origin of this adsorption.

Keywords: adsorption, nano-ions, solid-liquid interface, superchaotropicity

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Authors: Dilek Ozturk, Narin Ozturk, Zeliha Pala Kara, Engin Kaptan, Serap Sancar Bas, Nurten Ozsoy, Alper Okyar

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Most physiological processes oscillate in a rhythmic manner in mammals including metabolism and energy homeostasis, locomotor activity, hormone secretion, immune and endocrine system functions. Endocrine body rhythms are tightly regulated by the circadian timing system. The hypothalamic-pituitary-thyroid (HPT) axis is under circadian control at multiple levels from hypothalamus to thyroid gland. Since circadian timing system controls a variety of biological functions in mammals, circadian rhythms of biological functions may modify the drug tolerability/toxicity depending on the dosing time. Selective mTOR (mammalian target of rapamycin) inhibitor everolimus is an immunosuppressant and anticancer agent that is active against many cancers. It was also found to be active in medullary thyroid cancer. The aim of this study was to investigate the dosing time-dependent toxicity of everolimus on the thyroid gland and hormones in mice. Healthy C57BL/6J mice were synchronized with 12h:12h Light-Dark cycle (LD12:12, with Zeitgeber Time 0 – ZT0 – corresponding to Light onset). Everolimus was administered to male (5 mg/kg/day) and female mice (15 mg/kg/day) orally at ZT1-rest period- and ZT13-activity period- for 4 weeks; body weight loss, clinical signs and possible changes in serum thyroid hormone levels (TSH and free T4) were examined. Histological alterations in the thyroid gland were evaluated according to the following criteria: follicular size, colloid density and viscidity, height of the follicular epithelium and the presence of necrotic cells. The statistical significance between differences was analyzed with ANOVA. Study findings included everolimus-related diarrhea, decreased activity, decreased body weight gains, alterations in serum TSH levels, and histopathological changes in thyroid gland. Decreases in mean body weight gains were more evident in mice treated at ZT1 as compared to ZT13 (p < 0.001, for both sexes). Control tissue sections of thyroid glands exhibited well-organized histoarchitecture when compared to everolimus-treated groups. Everolimus caused histopathological alterations in thyroid glands in male (5 mg/kg, slightly) and female mice (15 mg/kg; p < 0.01 for both ZT as compared to their controls) irrespective of dosing-time. TSH levels were slightly decreased upon everolimus treatment at ZT13 in both males and females. Conversely, increases in TSH levels were observed when everolimus treated at ZT1 in both males (5 mg/kg; p < 0.05) and females (15 mg/kg; slightly). No statistically significant alterations in serum free T4 levels were observed. TSH and free T4 is clinically important thyroid hormones since a number of disease states have been linked to alterations in these hormones. Serum free T4 levels within the normal ranges in the presence of abnormal serum TSH levels in everolimus treated mice may suggest subclinical thyroid disease which may have repercussions on the cardiovascular system, as well as on other organs and systems. Our study has revealed the histological damage on thyroid gland induced by subacute everolimus administration, this effect was irrespective of dosing time. However, based on the body weight changes and clinical signs upon everolimus treatment, tolerability for the drug was best following dosing at ZT13 in both male and females. Yet, effects of everolimus on thyroid functions may deserve further studies regarding their clinical importance and chronotoxicity.

Keywords: circadian rhythm, chronotoxicity, everolimus, thyroid gland, thyroid hormones

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Authors: Pear-Rarin Leelakunakorn, Patompong Satapornpong

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Introduction: Dapsone is an anti-inflammatory and antibiotic drug that was widely used for the treatment of leprosy, acne fulminans, and dermatitis herpetiformis (DH). However, dapsone is the main cause that triggers severe cutaneous adverse reactions (SCARs), with a possibility of 0.4 to 3.6% of patients after initiating treatment. In fact, the mortality rate of dapsone-induced SCARs is approximately 9.9%. In previous studies, HLA-B*13:01 was strongly associated with dapsone-induced SCARs in Han Chinese, Thais, and Koreans. Nevertheless, the distribution of HLA-B*13:01 marker in each population might differ. Moreover, there were found that the association between HLA-C*03:04 and dapsone hypersensitivity syndrome in Han Chinese leprosy patients by OR = 9.00 and p-value = 2.23×10⁻¹⁹. Objective: The aim of this study was to investigate the distribution of HLA-C* 03:04 in Thailand's healthy population. Method: A total of 350 participants were HLA-C genotyping used sequence-specific oligonucleotides (PCR-SSOs). This study was approved by the Ethics Committee of Rangsit University Result : The most frequency of HLA -C alleles in Thais, consist of HLA -C* 01:02 (17.00 %), -C*08:01 (11.00%) , -C*07:02 (10.70%) , -C* 03:04 ( 9.10%) , -C* 03:02 (8.00%) , -C* 07:01 (6.30%), -C* 07:04 (4.60%), -C* 04:01 (4.40%) ,-C* 12:02 ( 4.30% ) ,and -C* 04:03(3.90%). Interestingly, HLA -C* 03:04 allele was similar to the distribution among Thais and other populations such as Eastern Europe (6.09%), Vietnam (7.42% ), East Croatia (2.25%), and Han Chinese (11.70%). Conclusion: Consequently, HLA-C*03:04 might serve as a pharmacogenetic marker for screening prior to initiation therapy with dapsone for prevention of dapsone-induced SCARs in Thai population.

Keywords: HLA-C*03:04, SCARs, thai population, allele frequency

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Authors: Kalin Ivanov, Stanislava Ivanova

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Actoprotectors are substances with hight performance enchasing potential and hight antioxidant activity. Most of these drugs have been developed in USSR for military medicine purposes. Based on their chemical composition actoprotectors could be classified into three categories: benzimidazole derivatives (ethomersol, bemitil); adamantane derivatives (bromantane), other chemical classes. First data for intake of actoprotectors from professional athletes is from 1980. The daily intake of actoprotectors demonstrate many benefits for athletes like: positive effect on the efficiency of physical work, antihypoxic effects, antioxidant effects, nootropic effects, rapid recovery. Since 1997, bromantane is considered as doping. This is a result of Summer Olympic Games in Athlanta (1996) when several Russian athletes tested positive for bramantane. Even the drug is safe for athletes health its use is considered as violation of anti- doping rules. More than 37 years bemetil has been used by professional athletes with no risk but currently it is included in WADA monitoring programme for 2018. Current perspectives are that most used actoprotectors would be considered as doping. Many clinical studies have confirmed that intake of bemitil and bromantan demonstrate positive influence on the physical work capacity but data for other actoprotectors like chlodantane, ademol, ethomersol is limited.

Keywords: actoprotector, sport, doping, bemitil

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Authors: Gerrit Ter Haar, Thorsten Becker, Deborah Blaine

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The Additive Manufacturing (AM) process of Selective Laser Melting (SLM) has seen an exponential growth in sales and development in the past fifteen years. Whereas the capability of SLM was initially limited to rapid prototyping, progress in research and development (R&D) has allowed SLM to be capable of fully functional parts. This technology is still at a primitive stage and technical knowledge of the vast number of variables influencing final part quality is limited. Ongoing research and development of the sensitive printing process and post processes is of utmost importance in order to qualify SLM parts to meet international standards. Quality concerns in Ti-6Al-4V manufactured through SLM has been identified, which include: high residual stresses, part porosity, low ductility and anisotropic mechanical properties. Whereas significant quality improvements have been made through optimising printing parameters, research indicates as-produced part ductility to be a major limiting factor when compared to its wrought counterpart. This study aims at achieving an in-depth understanding of the underlining links between SLM produced Ti-6Al-4V microstructure and its mechanical properties. Knowledge of microstructural transformation kinetics of Ti-6Al-4V allows for the optimisation of post-process heat treatments thereby achieving the required process route to manufacture high quality SLM produced Ti-6Al-4V parts. Experimental methods used to evaluate the kinematics of microstructural transformation of SLM Ti-6Al-4V are: optical microscopy and electron backscatter diffraction. Results show that a low-temperature heat treatment is capable of transforming the as-produced, martensitic microstructure into a duel-phase microstructure exhibiting both a high strength and improved ductility. Furthermore, isotropy of mechanical properties can be achieved through certain annealing routes. Mechanical properties identical to that of wrought Ti-6Al-4V can, therefore, be achieved through an optimised process route.

Keywords: EBSD analysis, heat treatments, microstructural characterisation, selective laser melting, tensile behaviour, Ti-6Al-4V

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Authors: Sachin Saxena, Manju Srivastava

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The present study describes a stable, highly sensitive and selective analytical sensor. Fe-BTC was synthesized at room temperature using the noble Iron-trimesate system. The high surface area of as synthesized Fe-BTC proved MOFs as ideal modifiers for glassy carbon electrode. The characterization techniques such as TGA, XRD, FT-IR, BET (BET surface area= 1125 m2/gm) analysis explained the electrocatalytic behaviour of Fe-BTC towards these two drugs. The material formed is cost effective and exhibit higher catalytic behaviour towards analyte systems. The synergism between synthesized Fe-BTC and electroanalytical techniques helped in developing a highly sensitive analytical method for studying the redox fate of ARP and RZ, respectively. Cyclic voltammetry of ferricyanide system proved Fe-BTC/GCE with an increase in 132% enhancement in peak current value as compared to that of GCE. The response characteristics of cyclic voltammetry (CV) and square wave voltammetry (SWV) revealed that the ARP and RZ could be effectively accumulated at Fe-BTC/GCE. On the basis of the electrochemical measurements, electrode dynamics parameters have been evaluated. Present study opens up new field of applications of MOFs modified GCE for drug sensing.

Keywords: MOFs, anti-psychotic, electrochemical sensor, anti-migraine drugs

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Authors: Mina Rahmani Pour

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Negative consequences of unemployment are: increasing age at marriage, addiction, depression, drug trafficking, divorce, immigration, elite, frustration, delinquency, theft, murder, etc., has led to addressing the issue of employment by economic planners, public authorities, chief executive economic conditions in different countries and different time is important. All countries are faced with the problem of unemployment. By identifying the influential factors of occupational employment and employing strengths in the basic steps can be taken to reduce unemployment. In this study, the most significant factors affecting employment has identified 12 variables based on interviews conducted Choose Vtasyrafzaysh engaged in three main business is discussed. DRGAM next question the 8 expert ministry to respond to it is distributed and for weight Horns AZFN Shannon entropy and the ranking criteria of the (SAW, TOPSIS) used. According to the results of the above methods are not compatible with each other, to reach a general consensus on the rating criteria of the technique of integrating (POSET) involving average, Borda, copeland is used. Ultimately, there is no difference between the employments in the economic sector jobs of increased employment.

Keywords: employment, effective techniques, SAW, TOPSIS

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Authors: Donna M. Morrison, Lambert Chester, Coretta A. N. Samuels, David R. Ledoux

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A survey was conducted in the five rice-growing regions in Guyana to determine the presence of aflatoxins in multiple fractions of rice in June/October 2015 growing season. The fractions were paddy, steamed paddy, cargo rice, white rice and parboiled rice. Samples were analyzed by High Performance Liquid Chromatography. A subset of the samples was further analyzed by enzyme-linked immunosorbent assay (ELISA) for concurrence. All analyses were conducted at the University of Missouri, USA. Of the 186 samples tested, 16 had aflatoxin concentrations greater than 20 ppb the recommended limit for aflatoxins in food according to the United States Food and Drug Administration. An additional three samples had aflatoxin B₁ concentrations greater than the European Union Commission maximum levels for aflatoxin B₁ in rice at 5 µg/kg and total aflatoxins (B₁, B₂, G₁ and G₂) at 10 µg/kg. The survey indicates that there is no widespread aflatoxin problem in rice in Guyana. The incidence of aflatoxins appears to be localized.

Keywords: aflatoxin, enzyme-linked immunosorbent assay (ELISA), high-performance liquid chromatography (HPLC), rice fractions

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Authors: Jyh-Cheng Chen, Tai-Jing Wang, Yun-Wei Lin

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Astaxanthin has been demonstrated to exhibit a wide range of beneficial effects including anti-inflammatory and anti-cancer properties. However, the molecular mechanism of astaxanthin-induced cytotoxicity in non-small cell lung cancer (NSCLC) cells has not been identified. Rad51 plays a central role in homologous recombination and high levels of Rad51 expression are observed in chemo- or radioresistant carcinomas. In this study, astaxanthin treatment inhibited cell viability and proliferation of two NSCLC cells, A549 and H1703. Treatment with astaxanthin decreased Rad51 expression and phospho-AKT protein level in a time and dose-dependent manner. Furthermore, expression of constitutively active AKT (AKT-CA) vector significantly rescued the decreased Rad51 protein and mRNA levels in astaxanthin-treated NSCLC cells. Combined treatment with PI3K inhibitors (LY294002 or wortmannin) and astaxanthin further decreased the Rad51 expression in NSCLC cells. Knockdown of Rad51 enhanced astaxanthin-induced cytotoxicity and growth inhibition in NSCLC cells. These findings may have implications for the rational design of future drug regimens incorporating astaxanthin for the treatment of NSCLC.

Keywords: astaxanthin, cytotoxicity, AKT, non-small cell lung cancer, PI3K

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Authors: S. Mamoucha, N.Tsafantakis, T. Ioannidis, S. Chatzipanagiotou, C. Nikolaou, L. Skaltsounis, N. Fokialakis, N. Christodoulakis

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Introduction: Pistacia lentiscus L. (well known as Mastic tree) is an evergreen sclerophyllous shrub that extensively thrives in the eastern Mediterranean area yet only the trees cultivated in the southern region of the Greek island Chios produces mastic resin. Different parts of P. lentiscus L. var. chia have been used in folk medicine for various purposes, such as tonic, aphrodisiac, antiseptic, antihypertensive and management of dental, gastrointestinal, liver, urinary, and respiratory tract disorders. Several studies have focused on the antibacterial activity of its resin (gum) and its essential oil. However, there is no study combining anatomy of the plant organs, phytochemical profile, and antibacterial screening of the plant. In our attempt to discover novel bioactive metabolites from the mastic tree, we screened its antibacterial activity not only against ATCC strains but also against clinical, resistant strains. Materials-methods: Leaves were investigated using Transmission (ΤΕΜ) and Scanning Εlectron Microscopy (SEM). Histochemical tests were performed on fresh and fixed tissue. Extracts prepared from dried, powdered leaves using 3 different solvents (DCM, MeOH and H2O) the waste water obtained after a hydrodistillation process for essential oil production were screened for their phytochemical content and antibacterial activity. Μetabolite profiling of polar and non-polar extracts was recorded by GC-MS and LC-HRMS techniques and analyzed using in-house and commercial libraries. The antibacterial screening was performed against Staphylococcus aureus ATCC25923, Escherichia coli ATCC25922, Pseudomonas aeruginosa ATCC27853 and against clinical, resistant strains Methicillin-resistant S. aureus (MRSA), Carbapenem-Resistant Metallo-β-Lactamase (carbapenemase) P. aeruginosa (VIM), Klebsiella pneumoniae carbapenemases (KPCs) and Acinetobacter baumanii resistant strains. The antibacterial activity was tested by the Kirby Bauer and the Agar Well Diffusion method. The zone of inhibition (ZI) of each extract was measured and compared with those of common antibiotics. Results: Leaf is compact with inosclereids and numerous idioblasts containing a globular, spiny crystal. The major nerves of the leaf contain a resin duct. Mesophyll cells showed accumulation of osmiophillic metabolites. Histochemical treatments defined secondary metabolites in subcellular localization. The phytochemical investigation revealed the presence of a large number of secondary metabolites, belonging to different chemical groups, such as terpenoids, phenolic compounds (mainly myricetin, kaempferol and quercetin glycosides), phenolic, and fatty acids. Among the extracts, the hydrostillation wastewater achieved the best results against most of the bacteria tested. MRSA, VIM and A. baumanii were inhibited. Conclusion: Extracts from plants have recently been of great interest with respect to their antimicrobial activity. Their use emerged from a growing tendency to replace synthetic antimicrobial agents with natural ones. Leaves of P. lentiscus L. var. chia showed a high antimicrobial activity even against drug - resistant bacteria. Future prospects concern the better understanding of mode of action of the antibacterial activity, the isolation of the most bioactive constituents and the clarification if the activity is related to a single compound or to the synergistic effect of several ones.

Keywords: antibacterial screening, leaf anatomy, phytochemical profile, Pistacia lentiscus var. chia

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Authors: Laxman H. Surwase, Lalit V. Sonawane, Bhagwat N. Poul

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A simple stability indicating high performance liquid chromatographic method has been developed for the simultaneous determination of Levosalbutamol Sulphate and Ipratropium Bromide in bulk and pharmaceutical dosage form using reverse phase Zorbax Eclipse Plus C8 column (250mm×4.6mm), with mobile phase phosphate buffer (0.05M KH2PO4): acetonitrile (55:45v/v) pH 3.5 adjusted with ortho-phosphoric acid, the flow rate was 1.0 mL/min and the detection was carried at 212 nm. The retention times of Levosalbutamol Sulphate and Ipratropium Bromide were 2.2007 and 2.6611 min respectively. The correlation coefficient of Levosalbutamol Sulphate and Ipratropium Bromide was found to be 0.997 and 0.998.Calibration plots were linear over the concentration ranges 10-100µg/mL for both Levosalbutamol Sulphate and Ipratropium Bromide. The LOD and LOQ of Levosalbutamol Sulphate were 2.520µg/mL and 7.638µg/mL while for Ipratropium Bromide was 1.201µg/mL and 3.640 µg/mL. The accuracy of the proposed method was determined by recovery studies and found to be 100.15% for Levosalbutamol Sulphate and 100.19% for Ipratropium Bromide respectively. The method was validated for accuracy, linearity, sensitivity, precision, robustness, system suitability. The proposed method could be utilized for routine analysis of Levosalbutamol Sulphate and Ipratropium Bromide in bulk and pharmaceutical capsule dosage form.

Keywords: levosalbutamol sulphate, ipratropium bromide, RP-HPLC, phosphate buffer, acetonitrile

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Authors: Milica Z. Karadzic, Lidija R. Jevric, Sanja Podunavac-Kuzmanovic, Strahinja Z. Kovacevic, Anamarija I. Mandic, Katarina Penov-Gasi, Andrea R. Nikolic, Aleksandar M. Okljesa

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In this study, a set of 29 newly synthesized steroid derivatives were investigated using reversed-phase high-performance liquid chromatography (RP-HPLC) as a first step in preselection of drug candidates. This analysis presents an experimental determination of chromatographic lipophilicity, and it was conducted to obtain physicochemical characterization of these molecules. As the most widely used bonded phases in RP-HPLC, octadecyl (C18) and octyl (C8) were used. Binary mixtures of water and acetonitrile or methanol were used as mobile phases. Obtained results were expressed as retention factor values logk and they were correlated with logP values. The results showed that both columns provide good estimations of the chromatographic lipophilicity of the molecules included in this study. This analysis was conducted in order to characterize newly synthesized steroid derivatives for further investigation regarding their antiproliferative and antimicrobial activity. This article is based upon work from COST Action (CM1306), supported by COST (European Cooperation in Science and Technology).

Keywords: antiproliferative activity, chromatographic lipophilicity, liquid chromatography, steroids

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Authors: Rufai Yakubu And Suleiman Kabiru

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Triterpenoids are a diverse class of secondary metabolites with potential antimicrobial properties. In this study, the crude extracts from ethyl acetate was obtained with ultrasonic extraction method. Using a combined chromatographic separation method to isolate squalene (1) stigmasterol (2), stigmasta-5,22-diene-3-ol acetate (3), γ-sitosterol (4), lupeol (5), taraxasterol (6), and betulinic acid (7) from ethyl acetate extracts. Ethyl acetate crude extracts and isolated compounds were both screened for antimicrobial activity and minimum inhibitory concentration (MIC). For ethyl acetate crude extracts with concentrations of (1.5, 0.75, 0.35, & 0.168 mg/mL) indicated marginal antibacterial activity with a range of 17, 20 and 14 mm zone of inhibition for Staphylococcus aureus, Escherichia coli and Candida albicans and lower minimum inhibitory concentrations ranges from 18.75 µg/ml to 150 µg/mL. Butulinic acid showed the highest activity against E. coli and C. albicans at 15 mm and 15 mm followed by Lupeol against S. aureus, E. coli and C. albicans at 13, 12, 12 mm. Moreso, no antimicrobial activity for both S. aureus and C. albicans with squalene except for E. coli which showed activity at 11 mm with 300 µg/mL (MIC). Thus, abundant triterpenoids in Deinbollia pinnata will be another centered area for antimicrobial drug discovery.

Keywords: triterpenoid, antimicrobial potentials, deinbollia pinnata, aerial parts

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Authors: Jaomai Tungsiripat, Patompong Satapornpong

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Allopurinol have been used to treat diseases that relating with the reduction of uric acid and be a treatment preventing the severity of, including gout, chronic kidney disease, chronic heart failure, and diabetes mellitus (type 2). However, allopurinol metabolites can cause a severe cutaneous adverse reaction (SCARs) consist of Drug Rash with Eosinophilia and Systemic Symptoms (DRESS) and Stevens-Johnson Syndrome(SJS)/Toxic Epidermal Necrolysis (TEN). Previous studies, we found only HLA-B*58:01 allele has a strongly association with allopurinol-induced SCARs in many populations: Han Chinese [P value = 4.7 x 10−24], European [P value <10−6], and Thai [P value <0.001].However, there was no update the frequency of HLA-B alleles and pharmacogenetics markers distribution in healthy Thais and support for screening before the initiation of treatment. The aim of this study was to investigate the prevalence of HLA-B*58:01 allele associated with allopurinol-induced SCARs in healthy Thai population. A retrospective study of 260 individual healthy subjects who living in Thailand. HLA-B were genotyped using sequence-specific oligonucleotides (PCR-SSOs).In this study, we identified the prevalence of HLA-B alleles consist ofHLA-B*46:01 (12.69%), HLA-B*15:02 (8.85%), HLA-B*13:01 (6.35%), HLA-B*40:01 (6.35%), HLA-B*38:02 (5.00%), HLA-B*51:01 (5.00%), HLA-B*58:01 (4.81%), HLA-B*44:03 (4.62%), HLA-B*18:01 (3.85%) and HLA-B*15:25 (3.08%). Therefore, the distribution of HLA-B*58:01 will support the clinical implementation and screening usage of allopurinol in Thai population.

Keywords: allopurinol, HLA-B*58: 01, Thai population, SCARs

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Authors: Laribi-Habchi Hasiba, Bouanane-Darenfed Amel, Drouiche Nadjib, Pausse André, Mameri Nabil

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Chitin, a linear 1, 4-linked N-acetyl-d-glucosamine (GlcNAc) polysaccharide is the major structural component of fungal cell walls, insect exoskeletons and shells of crustaceans. It is one of the most abundant naturally occurring polysaccharides and has attracted tremendous attention in the fields of agriculture, pharmacology and biotechnology. Each year, a vast amount of chitin waste is released from the aquatic food industry, where crustaceans (prawn, crab, Shrimp and lobster) constitute one of the main agricultural products. This creates a serious environmental problem. This linear polymer can be hydrolyzed by bases, acids or enzymes such as chitinase. In this context an extracellular chitinase (ChiA-65) was produced and purified from a newly isolated LHH100. Pure protein was obtained after heat treatment and ammonium sulphate precipitation followed by Sephacryl S-200 chromatography. Based on matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF/MS) analysis, the purified enzyme is a monomer with a molecular mass of 65,195.13 Da. The sequence of the 27 N-terminal residues of the mature ChiA-65 showed high homology with family-18 chitinases. Optimal activity was achieved at pH 4 and 75◦C. Among the inhibitors and metals tested p-chloromercuribenzoic acid, N-ethylmaleimide, Hg2+ and Hg + completelyinhibited enzyme activity. Chitinase activity was high on colloidal chitin, glycol chitin, glycol chitosane, chitotriose and chitooligosaccharide. Chitinase activity towards synthetic substrates in the order of p-NP-(GlcNAc) n (n = 2–4) was p-NP-(GlcNAc)2> p-NP-(GlcNAc)4> p-NP-(GlcNAc)3. Our results suggest that ChiA-65 preferentially hydrolyzed the second glycosidic link from the non-reducing end of (GlcNAc) n. ChiA-65 obeyed Michaelis Menten kinetics the Km and kcat values being 0.385 mg, colloidal chitin/ml and5000 s−1, respectively. ChiA-65 exhibited remarkable biochemical properties suggesting that this enzyme is suitable for bioconversion of chitin waste.

Keywords: Bacillus licheniformis LHH100, characterization, extracellular chitinase, purification

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Authors: Sandeep Pandey, Nimra Habib, Ranjana Singh, Abbas Ali Mahdi

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Leukemia is a malignancy of blood that mainly affects children and young adults; while advancement in the early diagnosis will have the potential to improve the outcome of diseases. A wide range of disease including leukemia shows inflammatory signals in their pathogenesis. In a pilot study conducted in our laboratory, 52 people were screened, of which 26 had leukemia and 26 were free from any kind of malignancy. We performed the estimation of the inflammatory cytokine Interleukin-8 and it was found significantly raised in all the leukemia patients concerning healthy volunteers who participated in the study. Flow cytometry had been performed for the confirmation of leukemia and further genomic, and proteomic, analyses of the sample revealed that IL-8 levels showed a positive correlation in patients with leukemia. The results had shown constitutive secretion of interleukin-8 by leukemia cells. So, our finding demonstrated that IL-8 is considered to have a role in the pathogenesis of leukemia, and quantification of IL-8 levels in leukemia conditions might be more useful and feasible in the clinical setting for the prediction of drug responses where it may represent a putative target for innovative diagnostic toward effective therapeutic approaches. However, further research explorations in this area are needed that include a greater number of patients with all different forms of leukemia, and estimating their IL-8 levels may hold the key for the additional predictive values on the recurrence of leukemia and its prognosis.

Keywords: T-ALL, IL-8, leukemia pathogenesis, cancer therapeutics

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Authors: T. A. Ajiboye

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This study examines the effects of health education programme on knowledge and prevention of cerebrovascular disease among hypertensive patients in University College Hospital, Ibadan. A quasi-experimental design was adopted for the study. 100 hypertensive patients were conveniently selected from general outpatient department in UCH. Data generated were analyzed using ANOVA at 0.05 alpha levels. The findings of the study revealed that health education programme significantly influenced both the knowledge of hypertensive patients (F=22.70; DF=1/99; p < .05) and their attitude (F=10.377; DF=1/99; p < .05) on cerebrovascular disease. Findings also discovered that health education programme significantly reduce the complication of hypertension to cerebrovascular disease (F= 16.41; DF=7/286; p < 0.05) among the hypertensive patients at UCH. Based on the findings, it is recommended that hypertensive patients should relieve themselves from stress, engage themselves on regular exercises, compliance with drug and diet regimes coupled with keeping up of regular appointment. Government should design health information that will center on hypertension and cerebrovascular disease so as to keep health and community development problems to the barest minimum. Finally, there should be provision of social amenities and recreational centers, as this will prevents hypertension problems.

Keywords: cerebrovascular disease, effectiveness, health education, hypertension, knowledge, prevention

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Authors: Daniel C. Bonzo

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Practical considerations lead to the use of unit of analysis within subjects, e.g., bleeding episodes or treatment-related adverse events, in rare disease settings. This is coupled with data augmentation techniques such as extrapolation to enlarge the subject base. In general, one can think about extrapolation of data as extending information and conclusions from one estimand to another estimand. This approach induces hierarchichal clustered data with varying cluster sizes. Extrapolation of clinical trial data is being accepted increasingly by regulatory agencies as a means of generating data in diverse situations during drug development process. Under certain circumstances, data can be extrapolated to a different population, a different but related indication, and different but similar product. We consider here the problem of estimation (point and interval) using a mixed-models approach under an extrapolation. It is proposed that estimators (point and interval) be constructed using weighting schemes for the clusters, e.g., equally weighted and with weights proportional to cluster size. Simulated data generated under varying scenarios are then used to evaluate the performance of this approach. In conclusion, the evaluation result showed that the approach is a useful means for improving statistical inference in rare disease settings and thus aids not only signal detection but risk-benefit evaluation as well.

Keywords: clustered data, estimand, extrapolation, mixed model

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Authors: Adewole Taiwo Adelabu

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The study investigated the factors militating the organization of intramural sports programs in secondary schools in Ekiti State, Nigeria. The purpose of the study was to identify the factors affecting the organization of sports in secondary schools and also to proffer possible solutions to these factors. The study employed the inferential statistics of chi-square (x2). Five research hypotheses were formulated. The population for the study was all the students in the government-owned secondary schools in Ekiti West Local Government of Ekiti State Nigeria. The sample for the study was 60 students in three schools within the local government selected through simple random sampling techniques. The instrument used for the study was a self-developed questionnaire by the researcher for data collection. The instrument was presented to experts and academicians in the field of Human Kinetics and Health Education for construct and content validation. A reliability test was conducted which involves 10 students who are not part of the study. The test-retest coefficient of 0.74 was obtained which attested to the fact that the instrument was reliable enough for the study. The validated questionnaire was administered to the students in their various schools by the researcher with the help of two research assistants; the questionnaires were filled and returned to the researcher immediately. The data collected were analyzed using the descriptive statistics of frequency count, percentage and mean to analyze demographic data in section A of the questionnaire, while inferential statistics of chi-square was used to test the hypotheses at 0.05 alpha level. The results of the study revealed that personnel, fund, schedule (time) were significant factors that affect the organization of intramural sport programs among students in secondary schools in Ekiti West Local Government Area of the State. The study also revealed that organization of intramural sports programs among students of secondary schools will improve and motivate students’ participation in sports beyond the local level. However, facilities and equipment is not a significant factor affecting the organization of intramural sports among secondary school students in Ekiti West Local Government Area.

Keywords: challenge, intramural sport, militating, programmes

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Authors: Hae Dun Kim, Joo Hyun Jang, Geu Rim Seo, Kyung Soo Ra, Hyung Joo Suh

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Lactuca sativa (lettuce) has been known for its medical property to relieve anxiety and nervous. This study was implemented to investigate sleep-promoting effects of the lettuce alcohol extract (LAE). Caffeine is widely used psychoactive substance known to induced wakefulness and insomnia to its consumers. In the present study, the sedative-hypnotic activity of the LAE was studied using the method of pentobarbital-induced sleep in the mouse model. The LAE was administrated to mice 30 min before the pentobarbital injection. The LAE prolonged the pentobarbital-induced sleep duration and decreased sleep latency. The effects of LAE were comparable to those of induced by diazepam. Another study was performed to examine whether LAE ameliorates caffeine-induced sleep disturbance in mice. Additionally, caffeine (10 mg/kg, p.o) delayed sleep onset and reduced sleep duration of mice. Conversely, LAE treatment (80 or 160 mg/kg, p.o), especially at 160 mg/kg, normalized the sleep disturbance induced by caffeine. LAE supplementation can counter the sleep disturbance induced by caffeine. These results suggest that LAE possess significant sedative-hypnotic activity, which supports the popular use of lettuce for treatment of insomnia and provide the basis for new drug discovery. Furthermore, these results demonstrate that the lettuce extract may be preferable for the treatment of insomnia.

Keywords: caffeine, Lactuca sativa, sleep duration, sleep latency

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Authors: Ihcen Khacheba, Amar Djeridane, Abdelkarim Kamli, Mohamed Yousfi

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Plant materials constitute an important source of natural bioactive molecules. Thus plants have been used from antiquity as sources of medicament against various diseases. These properties are usually attributed to secondary metabolites that are the subject of a lot of research in this field. This is particularly the case of phenolic compounds plants that are widely renowned in therapeutics as anti-inflammatories, enzyme inhibitors, and antioxidants, particularly flavonoïds. With the aim of acquiring a better knowledge of the secondary metabolism of the vegetable kingdom in the region of Laghouat and of the discovering of new natural therapeutics, 10 extracts from 5 Saharan plant species were submitted to chemical screening.The analysis of the preceding biological targets led to the evaluation of the biological activity of the extracts of the species Genista Corsica. The first step, consists in extracting and quantifying phenolic compounds. The second step has been devoted to stugying the effects of phenolic compounds on the kinetics catalyzed by two enzymes belonging to the class of hydrolase (the α-amylase and α-glucosidase) responsible for the digestion of sugars and finally we evaluate the antiantioxidant potential. The analysis results of phenolic extracts show clearly a low content of phenolic compounds in investigated plants. Average total phenolics ranged from 0.0017 to 11.35 mg equivalent gallic acid/g of the crude extract. Whereas the total flavonoids content lie between 0.0015 and 10.,96 mg/g equivalent of rutin. The results of the kinetic study of enzymatic reactions show that the extracts have inhibitory effects on both enzymes, with IC50 values ranging from 95.03 µg/ml to 1033.53 µg/ml for the α-amylase and 279.99 µg/ml to 1215.43 µg/ml for α-glucosidase whose greatest inhibition was found for the acetone extract of June (IC50 = 95.03 µg/ml). The results the antioxidant activity determined by ABTS, DPPH, and phosphomolybdenum tests clearly showed a good antioxidant capacity comparatively to antioxidants taken as reference the biological potential of these plants and could find their use in medicine to replace synthetic products.

Keywords: phenolic extracts, inhibition effect, α-amylase, α-glucosidase, antioxidant activity

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Authors: M. Krishna

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The study was intended to identify if scalp cooling therapy is effective on preventing chemotherapy-induced hair loss among cancer patients. Critical literature of non-randomized controlled trials was used to investigate whether scalp cooling therapy is effective on preventing chemotherapy-induced alopecia. The review identified that scalp cooling therapy is effective on preventing chemotherapy-induced alopecia. Most of the patients receiving chemotherapy experience alopecia. It is also perceived as the worst effect of chemotherapy. This may be severe and lead the patients to withdraw the chemo treatment. The image disturbance caused by alopecia will make the patient depressed and will lead to declined immunity. With the knowledge on effectiveness of scalp cooling therapy on preventing chemotherapy-induced alopecia, patient undergoing chemotherapy will not be hesitant to undergo the treatment. Patients are recommended to go through scalp cooling therapy every chemo cycle and the proper therapy duration is 30 minutes before, during chemo. The suggested duration of the scalp cooling therapy is 45-90 minutes for an effective and positive outcome. This finding is excluding other factors of alopecia such as menopause, therapeutic drugs, poor hair density, liver function problems, and drug regimes.

Keywords: alopecia, cancer, chemotherapy, scalp cooling therapy

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Authors: Parikshit Gogo, N. N. Dutta

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The oxidative enzymes specially laccase (benzenediol: oxygen oxidoreductase, E.C.1.10.3.2) from bacteria, fungi and plants have been playing an important role in green technologies due to their specific advantageous properties. Laccase from different sources and in different forms was used as a biocatalyst in many oxidation and conjugation reactions starting from phenol to hydrocarbons. Tea polyphenols and its derivatives attract the scientific community because of their potential use as antioxidants in food, pharmaceutical and cosmetic industries. Conjugate of polyphenols emerged as a novel materials which shows better stability and antioxidant properties in applied fields. The conjugation reaction of catechin with poly (allylamine) has been studied using free, immobilized and cross-linked enzyme crystals (CLEC) of laccase from Trametes versicolor with particular emphasis on the effect of pertinent variables and kinetic aspects of the reaction. The stability and antioxidant property of the conjugated product was improved as compared to the unconjugated tea polyphenols. The reaction was studied in 11 different solvents in order to deduce the solvent effect through an attempt to correlate the initial reaction rate with solvent properties such as hydrophobicity (logP), water solubility (logSw), electron pair acceptance (ETN) and donation abilities (DNN), polarisibility and dielectric constant which exhibit reasonable correlations. The study revealed, in general that polar solvents favour the initial reaction rate. The kinetics of the conjugation reaction conformed to the so-called Ping-Pong-Bi-Bi mechanism with catechin inhibition. The stability as well as activity of the CLEC was better than the free enzymes and immobilized laccase for practical application. In case of immobilized laccase system marginal diffusional limitation could be inferred from the experimental data. The kinetic parameters estimated by non-linear regression analysis were found to be KmPAA(mM) = 0.75, 1.8967 and Kmcat (mM) = 11.769, 15.1816 for free and immobilized laccase respectively. An attempt has been made to assess the activity of the laccase for the conjugation reaction in relation to other reactions such as dimerisation of ferulic acids and develop a protocol to enhance polyphenol antioxidant activity.

Keywords: laccase, catechin, conjugation reaction, antioxidant properties

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Authors: Mir Hussain Nawaz, Lyudmila Nedyalkova, Haizhong Zhu, Wael M. Rabeh

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In this study, we aim to biochemically and structurally characterize the interactions of human HK2 with the mitochondria in addition to the role of its N-terminal domain in catalysis and stability of the full-length enzyme. Here, we solved the crystal structure of human HK2 in complex with glucose and glucose-6-phosphate (PDB code: 2NZT), where it is a homodimer with catalytically active N- and C-terminal domains linked by a seven-turn α-helix. Different from the inactive N-terminal domains of isozymes 1 and 3, the N- domain of HK2 not only capable to catalyze a reaction but it is responsible for the thermodynamic stabilizes of the full-length enzyme. Deletion of first α-helix of the N-domain that binds to the mitochondria altered the stability and catalytic activity of the full-length HK2. In addition, we found the linker helix between the N- and C-terminal domains to play an important role in controlling the catalytic activity of the N-terminal domain. HK2 is a major step in the regulation of glucose metabolism in cancer making it an ideal target for the development of new anticancer therapeutics. Characterizing the structural and molecular mechanisms of human HK2 and its role in cancer metabolism will accelerate the design and development of new cancer therapeutics that are safe and cancer specific.

Keywords: cancer metabolism, enzymology, drug discovery, protein stability

Procedia PDF Downloads 262

Authors: Wenjun Zhang, Thao Thi Le, Dongyup Shin, Jong Min Kim

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Electrochemical hydrogen peroxide (H₂O₂) synthesis holds significant promise for decentralized environmental remediation through the electro-Fenton process. However, challenges persist, such as the absence of robust electrocatalysts for the selective two-electron oxygen reduction reaction (2e⁻ ORR) and the high cost and sluggish kinetics of conventional electro-Fenton systems in treating highly concentrated wastewater. This study introduces an efficient water treatment system for removing substantial quantities of organic pollutants using an advanced electro-Fenton system coupled with a high-valent NiO catalyst. By employing a precipitation method involving crystal facet and cation vacancy engineering, a trivalent Ni (Ni³⁺)-rich NiO catalyst with a (111)-domain-exposed crystal facet, named {111}-NivO, was synthesized. This catalyst exhibited a remarkable 96% selectivity and a high mass activity of 59 A g⁻¹ for H₂O₂ production, outperforming all previously reported Ni-based catalysts. Furthermore, an advanced electro-Fenton system, integrated with a flow cell for electrochemical H₂O₂ production, was utilized to achieve 100% removal of 50 ppm bisphenol A (BPA) in 200 mL of wastewater under heavy-duty conditions, reaching a superior rapid degradation rate (4 min, k = 1.125 min⁻¹), approximately 102 times faster than the conventional electro-Fenton system. The hyper-efficiency is attributed to the continuous and appropriate supply of H₂O₂, the provision of O₂, and the timely recycling of the electrolyte under high current density operation. This catalyst also demonstrated a 93% removal of total organic carbon after 2 hours of operation and can be applied for efficient removal of highly concentrated phenol pollutants from aqueous systems, which opens new avenues for wastewater treatment.

Keywords: hydrogen peroxide production, nickel oxides, crystal facet and cation vacancy engineering, wastewater treatment, flow cell, electro-Fenton

Procedia PDF Downloads 58

Authors: Avani Jain, S. Shelley, M. Indirani, Shilpa Kalal, Jaykanth Amalachandran

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Aim: To evaluate the prevalence of gall bladder dysfunction in patients with dyspepsia using In-House fatty meal cholescintigraphy. Materials & Methods: This study is a prospective cohort study. 59 healthy volunteers with no dyspeptic complaints and negative ultrasound and endoscopy were recruited in study. 61 patients having complaint of dyspepsia for duration of more than 6 months were included. All of them underwent 99mTc-Mebrofenin fatty meal cholescintigraphy following a standard protocol. Dynamic acquisitions were acquired for 120 minutes with an In-House fatty meal being given at 45th minute. Gall bladder emptying kinetics was determined with gall bladder ejection fractions (GBEF) calculated at 30minutes, 45minutes and at 60 minutes (30min, 45min & 60 min). Standardization of fatty meal was done for volunteers. Receiver operating characteristic (ROC) analysis was used assess the diagnostic accuracy of 3 time points (30min, 45min & 60 min) used for measuring gall bladder emptying. On the basis of cut off derived from volunteers, the patients were assessed for gall bladder dysfunction. Results: In volunteers, the GBEF at 30 min was 74.42±8.26 % (mean ±SD), at 45 min was 82.61 ± 6.5 % and at 60 min was 89.37±4.48%, compared to patients where at 30min it was 33.73±22.87%, at 45 min it was 43.03±26.97% and at 60 min it was 51.85±29.60%. The lower limit of GBEF in volunteers at 30 min was 60%, 45 min was 69% and at 60 min was 81%. ROC analysis showed that area under curve was largest for 30 min GBEF (0.952; 95% CI = 0.914-0.989) and that all the 3 measures were statistically significant (p < 0.005). Majority of the volunteers had 74% of gall bladder emptying by 30 minutes; hence it was taken as an optimum cutoff time to assess gall bladder contraction. > 60% GBEF at 30 min post fatty meal was considered as normal and < 60% GBEF as indicative of gall bladder dysfunction. In patients, various causes for dyspepsia were identified: GB dysfunction (63.93%), Peptic ulcer (8.19 %), Gastroesophageal reflux disease (8.19%), Gastritis (4.91%). In 18.03% of cases GB dysfunction coexisted with other gastrointestinal conditions. The diagnosis of functional dyspepsia was made in 14.75% of cases. Conclusions: Gall bladder dysfunction contributes significantly to the causation of dyspepsia. It could coexist with various other gastrointestinal diseases. Fatty meal was well tolerated and devoid of any side effects. Many patients who are labeled as functional dyspeptics could actually have gall bladder dysfunction. Hence as an adjunct to ultrasound and endoscopy, fatty meal cholescintigraphy can also be used as a screening modality in characterization of dyspepsia.

Keywords: in-house fatty meal, choescintigraphy, dyspepsia, gall bladder ejection fraction, functional dyspepsia

Procedia PDF Downloads 507

Authors: Sima Cheraghi Dehdezi, Nasser Hamdami

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Air-drying is the most widely employed method for preserving fruits and vegetables. Most of the dried products must be rehydrated by immersion in water prior to their use, so the study of rehydration kinetics in order to optimize rehydration phenomenon has great importance. Rehydration typically composes of three simultaneous processes: the imbibition of water into dried material, the swelling of the rehydrated products and the leaching of soluble solids to rehydration medium. In this research, squash (Cucurbita pepo) fruits were cut into 0.4 cm thick and 4 cm diameter slices. Then, squash slices were blanched in a steam chamber for 4 min. After cooling to room temperature, squash slices were dehydrated in a hot air dryer, under air flow 1.5 m/s and air temperature of 60°C up to moisture content of 0.1065 kg H2O per kg d.m. Dehydrated samples were kept in polyethylene bags and stored at 4°C. Squash slices with specified weight were rehydrated by immersion in distilled water at different temperatures (25, 50, and 75°C), various dry matter-water ratios (1:25, 1:50, and 1:100), which was agitated at 100 rpm. At specified time intervals, up to 300 min, the squash samples were removed from the water, and the weight, moisture content and rehydration indices of the sample were determined.The texture characteristics were examined over a 180 min period. The results showed that rehydration time and temperature had significant effects on moisture content, water absorption capacity (WAC), dry matter holding capacity (DHC), rehydration ability (RA), maximum force and stress in dried squash slices. Dry matter-water ratio had significant effect (p˂0.01) on all squash slice properties except DHC. Moisture content, WAC and RA of squash slices increased, whereas DHC and texture firmness (maximum force and stress) decreased with rehydration time. The maximum moisture content, WAC and RA and the minimum DHC, force and stress, were observed in squash slices rehydrated into 75°C water. The lowest moisture content, WAC and RA and the highest DHC, force and stress, were observed in squash slices immersed in water at 1:100 dry matter-water ratio. In general, for all rehydration conditions of squash slices, the highest water absorption rate occurred during the first minutes of process. Then, this rate decreased. The highest rehydration rate and amount of water absorption occurred in 75°C.

Keywords: dry matter-water ratio, squash, maximum force, rehydration ability

Procedia PDF Downloads 312

Authors: Raina J. Olsen, Andrew K. Gillespie, John W. Taylor, Cristian I. Contescu, Peter Pfeifer, James R. Morris

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While adsorbent surfaces such as graphite are known to increase the melting temperature of solid H2, this effect is normally rather small, increasing to 20 Kelvin (K) relative to 14 K in the bulk. An as-yet unidentified phase transition has been observed in a system of H2 adsorbed in a porous, locally graphitic, Saran carbon with sub-nanometer sized pores at temperatures (74-101 K) and pressures ( > 76 bar) well above the critical point of bulk H2 using hydrogen adsorption and neutron scattering experiments. Adsorption data shows a discontinuous pressure jump in the kinetics at 76 bar after nearly an hour of equilibration time, which is identified as an exothermic phase transition. This discontinuity is observed in the 87 K isotherm, but not the 77 K isotherm. At higher pressures, the measured isotherms show greater excess adsorption at 87 K than 77 K. Inelastic neutron scattering measurements also show a striking phase transition, with the amount of high angle scattering (corresponding to large momentum transfer/ large effective mass) increasing by up to a factor of 5 in the novel phase. During the course of the neutron scattering experiment, three of these reversible spectral phase transitions were observed to occur in response to only changes in sample temperature. The novel phase was observed by neutron scattering only at high H2 pressure (123 bar and 187 bar) and temperatures between 74-101 K in the sample of interest, but not at low pressure (30 bar), or in a control activated carbon at 186 bar of H2 pressure. Based on several of the more unusual observations, such as the slow equilibration and the presence of both an upper and lower temperature bound, a reasonable hypothesis is that this phase forms only in the presence of a high concentration of ortho-H2 (nuclear spin S=1). The increase in adsorption with temperature, temperatures which cross the lower temperature bound observed by neutron scattering, indicates that this novel phase is denser. Structural characterization data on the adsorbent shows that it may support a commensurate solid phase denser than those known to exist on graphite at much lower temperatures. Whatever this phase is eventually proven to be, these results show that surfaces can have a more striking effect on hydrogen phases than previously thought.

Keywords: adsorbed phases, hydrogen, neutron scattering, nuclear spin

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