scholarly journals Investigation of thermochemical Features of Gamma Irradiated Tryptophan Stereoisomers

2021 ◽  
Vol 66 (1) ◽  
Author(s):  
Ana Neacsu ◽  
Daniela Gheorghe ◽  
Victorita Tecuceanu ◽  
Stefan Perisanu

Abstract. In this work, the use of differential scanning calorimetry (DSC) is demonstrated as a powerful technique that can provide accurate thermodynamic property values of nutritional supplements such as tryptophan. Nutritional supplements require a decontamination procedure and irradiation appears as a promising technique for this purpose. The valuable properties of tryptophan for food and pharmaceutical industry as dietary supplement have led to increasing interest in its technological behaviour. L-, D- isomers and DL-racemic mixture of tryptophan irradiated and non-irradiated were studied by DSC. Irradiation was performed at room temperature with gamma radiations using a 137Cs source, the irradiation dose range was between 0.6- 10 kGy. Two steps decomposition pattern for both irradiated and non-irradiated samples up to 350 oC was found. Fourier transform infrared spectroscopic studies were performed. The obtained results indicate that the irradiation process does not inhibit the thermal properties of tryptophan when irradiated up to 10 kGy. The HPLC method was employed to evidence the degradation of the irradiated material.   Resumen. En este trabajo, se demuestra el uso de calorimetría diferencial de barrido (DSC) como una técnica poderosa que puede proporcionar valores precisos de propiedades termodinámicas de suplementos nutricionales como el triptófano. Los suplementos nutricionales requieren un procedimiento de descontaminación y la irradiación aparece como una técnica prometedora para este propósito. Las valiosas propiedades del triptófano para la industria alimentaria y farmacéutica como suplemento dietético han provocado un creciente interés por su comportamiento tecnológico. Los isómeros L-, D- y la mezcla racémica DL- de triptófano irradiado y no irradiado fueron estudiados por DSC. La irradiación se realizó a temperatura ambiente con radiaciones gamma utilizando una fuente de 137Cs, el rango de dosis de irradiación estuvo entre 0.6 - 10 kGy. Se encontró un patrón de descomposición de dos pasos para muestras irradiadas y no irradiadas hasta 350 ºC. Se realizaron estudios espectroscópicos de infrarrojos por la transformada de Fourier. Los resultados obtenidos indican que el proceso de irradiación no inhibe las propiedades térmicas del triptófano cuando se irradia hasta 10 kGy. Se empleó el método HPLC para evidenciar la degradación del material irradiado.

2015 ◽  
Vol 239 ◽  
pp. 98-109
Author(s):  
D. Singh ◽  
G.S. Mudahar ◽  
K.S. Thind ◽  
Hardev Singh Virk

The effects of gamma radiations on the optical, physical and structural properties of zinc lead borate xZnO-2xPbO-(1-3x)B2O3 and zinc lead borosilicate xZnO-2xPbO-1/2(1-3x)B2O3-1/2(1-3x)SiO2 glasses have been investigated. Differential Scanning Calorimetry (DSC), Ultraviolet-Visible (UV-Vis) and Fourier Transmission Infra-red (FTIR) spectroscopic techniques have been used to compare the properties of samples before and after gamma irradiation by a dose of 2.5 kGy. The variation of density, optical band gap (Eg), IR absorption bands and glass transition temperature (Tg) indicates that the structure of glasses changes due to irradiation. The radiation induced changes created by-ray in the optical, physical and thermal parameters in both the prepared series of glasses have been discussed for their possible application as radiation shielding material.


2013 ◽  
Vol 33 (9) ◽  
pp. 823-828 ◽  
Author(s):  
Carmina Menchaca-Campos ◽  
Gonzalo Martínez-Barrera ◽  
Héctor López-Valdivia ◽  
Héctor Carrasco ◽  
Alberto Álvarez-Castillo

Abstract Post-irradiation effects on nylon 6,12 crystalline fibers gamma-irradiated 6 years previously (6YI) were studied, including thermal stability and morphology; their relationship with storage time was also studied. The results of these studies were compared with those obtained for non-irradiated (NI) and namely freshly irradiated (FI) crystalline fibers. The results include analyses like thermogravimetric analysis (TGA), differential thermal analysis (DTA), scanning electron microscopy (SEM) and optical images for (6YI and FI) both kinds of nylon 6,12 fibers. The results showed that the most prominent effect is related to the reaction progress. The chain scission and/or crosslinking mechanisms, as well as the free radicals, allow proceeding with the reaction, and consequently, changes on the properties of the FI samples. The melting point, degree of crystallinity, degradation temperature and morphology prove that additional chemical reactions and surface modifications keep occurring in the fibers long after the irradiation process has ended. With storage time, the surface becomes rougher, the color turns yellowish, the melting point diminishes and the degree of crystallinity increases.


Author(s):  
Mateusz Gołdyn ◽  
Anna Komasa ◽  
Mateusz Pawlaczyk ◽  
Aneta Lewandowska ◽  
Elżbieta Bartoszak-Adamska

The study of various forms of pharmaceutical substances with specific physicochemical properties suitable for putting them on the market is one of the elements of research in the pharmaceutical industry. A large proportion of active pharmaceutical ingredients (APIs) occur in the salt form. The use of an acidic coformer with a given structure and a suitable pK a value towards purine alkaloids containing a basic imidazole N atom can lead to salt formation. In this work, 2,6-dihydroxybenzoic acid (26DHBA) was used for cocrystallization of theobromine (TBR) and caffeine (CAF). Two novel salts, namely, theobrominium 2,6-dihydroxybenzoate, C7H9N4O2 +·C7H5O4 − (I), and caffeinium 2,6-dihydroxybenzoate, C8H11N4O2 +·C7H5O4 − (II), were synthesized. Both salts were obtained independently by slow evaporation from solution, by neat grinding and also by microwave-assisted slurry cocrystallization. Powder X-ray diffraction measurements proved the formation of the new substances. Single-crystal X-ray diffraction studies confirmed proton transfer between the given alkaloid and 26DHBA, and the formation of N—H...O hydrogen bonds in both I and II. Unlike the caffeine cations in II, the theobromine cations in I are paired by noncovalent N—H...O=C interactions and a cyclic array is observed. As expected, the two hydroxy groups in the 26DHBA anion in both salts are involved in two intramolecular O—H...O hydrogen bonds. C—H...O and π–π interactions further stabilize the crystal structures of both compounds. Steady-state UV–Vis spectroscopy showed changes in the water solubility of xanthines after ionizable complex formation. The obtained salts I and II were also characterized by theoretical calculations, Fourier-transform IR spectroscopy (FT–IR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and elemental analysis.


2017 ◽  
Vol 100 (1) ◽  
pp. 65-73
Author(s):  
Nilusha Padivitage ◽  
Satish Kumar ◽  
Abu Rustum

Abstract Afoxolaner is a new antiparasitic molecule from the isoxazoline family that acts on insect acarine g-aminobutyric acid and glutamate receptors. Afoxolaner is a racemic mixture, which has a chiral center at the isoxazoline ring. A reversed-phase chiral HPLC method has been developed to determine the chiral purity of bulk batches of (S)-enantiomer in afoxolaner for the first time. This method can also be used to verifythat afoxolaner is a racemic mixture, which was demonstrated by specific rotation. ChromSword, an artificial intelligence method development tool, was used for initial method development. The column selected for the final method was CHIRALPAK AD-RH (150 × 4.6 mm, 5 μm particle size), maintained at 45°C, and isocratic elution using water–isopropanol–acetonitrile (40 + 50 + 10, v/v/v) as the mobile phasewith a detection wavelength of 312 nm. The run time for the method was 11 min. The resolution and selectivity factors of the two enantiomers were 2.3 and 1.24, respectively. LOQ and LOD of the method were 1.6 and 0.8 μg/mL, respectively. This method was appropriately validated according to International Conference on Harmonization guidelines for its intended use.


Author(s):  
SAMIULLAH ◽  
SYED UMER JAN ◽  
RAHMAN GUL ◽  
SYED JALALUDIN ◽  
ASMATHULLAH

Objective: This study was conducted to design a transdermal dosage form of pseudoephedrine HCL and to evaluate its release under controlled rates for sustained transdermal delivery of Pseudoephedrine. Methods: Transdermal patches were prepared by the casting evaporation method. Utilizing eudragit RL100. Patches were characterized by physical appearance, moisture content, thickness, weight variation, folding endurance, tensile strength and stability studies. Fourier transform infrared spectroscopic studies (FTIR), differential scanning calorimetry analysis (SCA) and XRD studies. Four different permeation enhancer (Tween 20, thymus oil, castor oil and eucalyptus oil) was employed. In vitro release of drugs was done in the dissolution paddle apparatus. Release studies were performed in distilled water at 37 °C. Scanning electron microscope studies were performed before and after the drug. Results: Transdermal patches with enhancers were formulated successfully with a concentration of 1% (W/V). The patches indicated stable physicochemical characteristics. FTIR, SCA and XRD Studies showed that there were no physical and chemical interactions between excipients and drugs. Results of in vitro permeation studies showed that enhancers used in this study increased drug released. The enhancers showed faster released than no enhancer. This arrangement can be shown as Tween>Eucalyptus oil>Thymus oil and castor oil. Formulation F2 is optimized among all formulations showed an 83.3% release. Conclusion: Transdermal patches of pseudoephedrine were successfully developed by using pseudo epinephrine HCL. These patches proved to be very useful for therapeutic purposes in the pharmaceutical industry without making the patients unconscious, unlike the trivial methods of treatment.


Author(s):  
Dileep M S ◽  
Suresh Kumar H.M. ◽  
Sindhu Tilak

The thiourea doped lithium sulfate single crystal was grown by solution growth slow evaporation technique. The unit cell parameters of the grown crystal determined by X-ray diffraction studies indicated that the crystal belongs to a monoclinic crystal system with noncentrosymmetric space group P2. UV-visible spectral study signified that the crystal possesses an energy gap of 4.54 eV with 68% transparency in the visible region. The grown crystals were irradiated by Co-60 gamma radiations with different doses of 10 kGy, 30 kGy & 50 kGy and studied irradiation effect on powder XRD, dielectric properties, mechanical hardness, linear transmittance and second harmonic generation of the crystal. It is observed that the crystallite size, energy gap and transparency are decreased; whereas, the dielectric constant, AC conductivity, microhardness and SHG efficiency are increased upon an increase in radiation dose.


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