Displaying publications 1 - 20 of 116 in total

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  1. Ramimoghadam D, Bagheri S, Abd Hamid SB
    Biomed Res Int, 2014;2014:205636.
    PMID: 25126547 DOI: 10.1155/2014/205636
    Anatase titanium dioxide nanoparticles (TiO2-NPs) were synthesized by sol-gel method using rice straw as a soft biotemplate. Rice straw, as a lignocellulosic waste material, is a biomass feedstock which is globally produced in high rate and could be utilized in an innovative approach to manufacture a value-added product. Rice straw as a reliable biotemplate has been used in the sol-gel method to synthesize ultrasmall sizes of TiO2-NPs with high potential application in photocatalysis. The physicochemical properties of titanium dioxide nanoparticles were investigated by a number of techniques such as X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analysis (TGA), ultraviolet visible spectra (UV-Vis), and surface area and pore size analysis. All results consensually confirmed that particle sizes of synthesized titanium dioxide were template-dependent, representing decrease in the nanoparticles sizes with increase of biotemplate concentration. Titanium dioxide nanoparticles as small as 13.0 ± 3.3 nm were obtained under our experimental conditions. Additionally, surface area and porosity of synthesized TiO2-NPs have been enhanced by increasing rice straw amount which results in surface modification of nanoparticles and potential application in photocatalysis.
    Matched MeSH terms: Spectrum Analysis, Raman
  2. Yeu TH, Omar IS, Sani SFA, Pathmanathan D, Goh BT, Ravindran N, et al.
    Appl Spectrosc, 2023 Jul;77(7):723-733.
    PMID: 37357678 DOI: 10.1177/00037028231182721
    Obesity is strongly linked with increased risk and poorer prognosis of endometrial cancer (EC). Cancer-associated fibroblasts (CAFs) are activated fibroblasts that form a large component of the tumor microenvironment and undergo metabolic reprogramming to provide critical metabolites for tumor growth. However, it is still unknown how obesity, characterized by a surplus of free fatty acids drives the modifications of CAFs lipid metabolism which may provide the mechanistic link between obesity and EC progression. The present study aims to evaluate the utility of Raman spectroscopy, an emerging nondestructive analytical tool to detect signature changes in lipid metabolites of CAFs from EC patients with varying body mass index. We established primary cultures of fibroblasts from human EC tissues, and CAFs of overweight/obese and nonobese women using antibody-conjugated magnetic beads isolation. These homogeneous fibroblast cultures expressed fibroblast markers, including α-smooth muscle actin and vimentin. Analysis was made in the Raman spectra region best associated with cancer progression biochemical changes in lipids (600-1800 cm-1 and 2800-3200 cm-1). Direct band analysis and ratiometric analysis were conducted to extract information from the Raman spectrum. Present results demonstrated minor shifts in the CH2 symmetric stretch of lipids at 2879 cm-1 and CH3 asymmetric stretching from protein at 2932 cm-1 in the overweight/obese CAFS compared to nonobese CAFs, indicating increased lipid content and a higher degree of lipid saturation. Principal component analysis showed that CAFs from overweight/obese and nonobese EC patients can be clearly distinguished indicating the capability of Raman spectroscopy to detect changes in biochemical components. Our results suggest Raman spectroscopy supported by chemometric analysis is a reliable technique for characterizing metabolic changes in clinical samples, providing an insight into obesity-driven alteration in CAFs, a critical stromal component during EC tumorigenesis.
    Matched MeSH terms: Spectrum Analysis, Raman
  3. Ridhuan NS, Razak KA, Lockman Z, Abdul Aziz A
    PLoS One, 2012;7(11):e50405.
    PMID: 23189199 DOI: 10.1371/journal.pone.0050405
    In this study, zinc oxide (ZnO) nanorod arrays were synthesized using a simple hydrothermal reaction on ZnO seeds/n-silicon substrate. Several parameters were studied, including the heat-treatment temperature to produce ZnO seeds, zinc nitrate concentration, pH of hydrothermal reaction solution, and hydrothermal reaction time. The optimum heat-treatment temperature to produce uniform nanosized ZnO seeds was 400°C. The nanorod dimensions depended on the hydrothermal reaction parameters. The optimum hydrothermal reaction parameters to produce blunt tip-like nanorods (770 nm long and 80 nm in top diameter) were 0.1 M zinc nitrate, pH 7, and 4 h of growth duration. Phase analysis studies showed that all ZnO nanorods exhibited a strong (002) peak. Thus, the ZnO nanorods grew in a c-axis preferred orientation. A strong ultraviolet (UV) emission peak was observed for ZnO nanorods grown under optimized parameters with a low, deep-level emission peak, which indicated high optical property and crystallinity of the nanorods. The produced ZnO nanorods were also tested for their UV-sensing properties. All samples responded to UV light but with different sensing characteristics. Such different responses could be attributed to the high surface-to-volume ratio of the nanorods that correlated with the final ZnO nanorods morphology formed at different synthesis parameters. The sample grown using optimum synthesis parameters showed the highest responsivity of 0.024 A/W for UV light at 375 nm under a 3 V bias.
    Matched MeSH terms: Spectrum Analysis, Raman
  4. Banihashemian SM, Periasamy V, Boon Tong G, Abdul Rahman S
    PLoS One, 2016;11(3):e0149488.
    PMID: 26999445 DOI: 10.1371/journal.pone.0149488
    Studying the effect of a magnetic field on oligonucleotide DNA can provide a novel DNA manipulation technique for potential application in bioengineering and medicine. In this work, the optical and electrochemical response of a 100 bases oligonucleotides DNA, cytosine-guanine (CG100), is investigated via exposure to different magnetic fields (250, 500, 750, and 1000 mT). As a result of the optical response of CG100 to the magnetic field, the ultra-violet-visible spectrum indicated a slight variation in the band gap of CG100 of about 0.3 eV. Raman spectroscopy showed a significant deviation in hydrogen and phosphate bonds' vibration after exposure to the magnetic field. Oligonucleotide DNA mobility was investigated in the external electric field using the gel electrophoresis technique, which revealed a small decrease in the migration of CG100 after exposure to the magnetic field.
    Matched MeSH terms: Spectrum Analysis, Raman/methods*
  5. Khanis NH, Ritikos R, Ahmad Kamal SA, Abdul Rahman S
    Materials (Basel), 2017 Jan 24;10(2).
    PMID: 28772460 DOI: 10.3390/ma10020102
    Nanostructured hydrogenated carbon nitride (CNx:H) thin films were synthesized on a crystal silicon substrate at low deposition temperature by radio-frequency plasma-enhanced chemical vapor deposition (PECVD). Methane and nitrogen were the precursor gases used in this deposition process. The effects of N₂ to the total gas flow rate ratio on the formation of CNx:H nanostructures were investigated. Field-emission scanning electron microscopy (FESEM), Auger electron spectroscopy (AES), Raman scattering, and Fourier transform of infrared spectroscopies (FTIR) were used to characterize the films. The atomic nitrogen to carbon ratio and sp² bonds in the film structure showed a strong influence on its growth rate, and its overall structure is strongly influenced by even small changes in the N₂:(N₂ + CH₄) ratio. The formation of fibrous CNx:H nanorod structures occurs at ratios of 0.7 and 0.75, which also shows improved surface hydrophobic characteristic. Analysis showed that significant presence of isonitrile bonds in a more ordered film structure were important criteria contributing to the formation of vertically-aligned nanorods. The hydrophobicity of the CNx:H surface improved with the enhancement in the vertical alignment and uniformity in the distribution of the fibrous nanorod structures.
    Matched MeSH terms: Spectrum Analysis, Raman
  6. Arunagiri C, Subashini A, Saranya M, Thomas Muthiah P, Thanigaimani K, Abdul Razak I
    PMID: 25084236 DOI: 10.1016/j.saa.2014.07.016
    The molecular structure of a new Schiff base, 2-[4-hydroxy benzylidene]-amino naphthalene (HBAN) has been examined by HF and B3LYP/6-311++G(d,p) calculations. The X-ray structure was determined in order to establish the conformation of the molecule. The compound, C17H13NO, crystallizes in the orthorhombic, P212121 space group with the cell dimension, a=6.2867(2), b=10.2108(3), c=19.2950(6) Å, α=β=γ=90° and z=4. The asymmetric unit contains a molecule of a Schiff base. A strong intermolecular O-H⋯N and a weak C-H⋯O hydrogen bonds stabilized the crystal structure. The vibrational spectra of HBAN have been calculated using density functional theoretical computation and compared with the experimental. The study is extended to the HOMO-LUMO analysis to calculate the energy gap (Δ), Ionization potential (I), Electron Affinity (A), Global Hardness (η), Chemical Potential (μ) and Global Electrophilicity (w). The calculated HOMO and LUMO energy reveals that the charge transfer occurs within the molecule.
    Matched MeSH terms: Spectrum Analysis, Raman
  7. Bradley DA, Siti Rozaila Z, Khandaker MU, Almugren KS, Meevasana W, Abdul Sani SF
    Appl Radiat Isot, 2019 May;147:105-112.
    PMID: 30852298 DOI: 10.1016/j.apradiso.2019.02.016
    We explore the utility of controlled low-doses (0.2-100 Gy) of photon irradiation as initiators of structural alteration in carbon-rich materials. To-date our work on carbon has focused on β-, x- and γ-irradiations and the monitoring of radiotherapeutic doses (from a few Gy up to some tens of Gy) on the basis of the thermoluminescence (TL) signal, also via Raman and X-ray photo-spectroscopy (XPS), providing analysis of the dose dependence of single-walled carbon nanotubes (SWCNT). The work has been extended herein to investigate possibilities for analysis of structural alterations in graphite-rich mixtures, use being made of two grades of graphite-rich pencil lead, 8H and 2B, both being in the form produced for mechanical pencils (propelling or clutch pencils). 2B has the greater graphite content (approaching 98 wt %), 8H being a mixture of C, O, Al and Si (with respective weight percentages 39.2, 38.2, 9.8 and 12.8). Working on media pre-annealed at 400 °C, both have subsequently been irradiated to penetrating photon-mediated doses. Raman spectroscopy analysis has been carried out using a 532 nm laser Raman spectrometer, while for samples irradiated to doses from 1 to 40 Gy, XPS spectra were acquired using Al Kα sources (hv ∼1400 eV); carbon KLL Auger peaks were acquired using 50 eV Pass Energy. At these relatively low doses, alterations in order-disorder are clearly observed, defect generation and internal annealing competing as dominating effects across the dose range.
    Matched MeSH terms: Spectrum Analysis, Raman
  8. Noroozi M, Zakaria A, Radiman S, Abdul Wahab Z
    PLoS One, 2016;11(4):e0152699.
    PMID: 27064575 DOI: 10.1371/journal.pone.0152699
    In this paper, we report how few layers graphene that can be produced in large quantity with low defect ratio from exfoliation of graphite by using a high intensity probe sonication in water containing liquid hand soap and PVP. It was founded that the graphene powder obtained by this simple exfoliation method after the heat treatment had an excellent exfoliation into a single or layered graphene sheets. The UV-visible spectroscopy, FESEM, TEM, X-ray powder diffraction and Raman spectroscopy was used to analyse the graphene product. The thermal diffusivity of the samples was analysed using a highly accurate thermal-wave cavity photothermal technique. The data obtained showed excellent enhancement in the thermal diffusivity of the graphene dispersion. This well-dispersed graphene was then used to fabricate an electrically conductive polymer-graphene film composite. The results demonstrated that this low cost and environmental friendly technique allowed to the production of high quality layered graphene sheets, improved the thermal and electrical properties. This may find use in the wide range of applications based on graphene.
    Matched MeSH terms: Spectrum Analysis, Raman
  9. Mustapa MA, Yuzir A, Latif AA, Ambran S, Abdullah N
    PMID: 38310743 DOI: 10.1016/j.saa.2024.123977
    A rapid, simple, sensitive, and selective point-of-care diagnosis tool kit is vital for detecting the coronavirus disease (COVID-19) based on the severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) strain. Currently, the reverse transcriptase-polymerase chain reaction (RT-PCR) is the best technique to detect the disease. Although a good sensitivity has been observed in RT-PCR, the isolation and screening process for high sample volume is limited due to the time-consuming and laborious work. This study introduced a nucleic acid-based surface-enhanced Raman scattering (SERS) sensor to detect the nucleocapsid gene (N-gene) of SARS-CoV-2. The Raman scattering signal was amplified using gold nanoparticles (AuNPs) possessing a rod-like morphology to improve the SERS effect, which was approximately 12-15 nm in diameter and 40-50 nm in length. These nanoparticles were functionalised with the single-stranded deoxyribonucleic acid (ssDNA) complemented with the N-gene. Furthermore, the study demonstrates method selectivity by strategically testing the same virus genome at different locations. This focused approach showcases the method's capability to discern specific genetic variations, ensuring accuracy in viral detection. A multivariate statistical analysis technique was then applied to analyse the raw SERS spectra data using the principal component analysis (PCA). An acceptable variance amount was demonstrated by the overall variance (82.4 %) for PC1 and PC2, which exceeded the desired value of 80 %. These results successfully revealed the hidden information in the raw SERS spectra data. The outcome suggested a more significant thymine base detection than other nitrogenous bases at wavenumbers 613, 779, 1219, 1345, and 1382 cm-1. Adenine was also less observed at 734 cm-1, and ssDNA-RNA hybridisations were presented in the ketone with amino base SERS bands in 1746, 1815, 1871, and 1971 cm-1 of the fingerprint. Overall, the N-gene could be detected as low as 0.1 nM within 10 mins of incubation time. This approach could be developed as an alternative point-of-care diagnosis tool kit to detect and monitor the COVID-19 disease.
    Matched MeSH terms: Spectrum Analysis, Raman/methods
  10. Ibrahim R, Hussein MZ, Yusof NA, Abu Bakar F
    Nanomaterials (Basel), 2019 Aug 31;9(9).
    PMID: 31480466 DOI: 10.3390/nano9091239
    Carbon nanotube-quicklime nanocomposites (CQNs) have been synthesized via the chemical vapor deposition (CVD) of n-hexane using a nickel metal catalyst supported on calcined carbonate stones at temperatures of 600-900 °C. The use of a Ni/CaO(10 wt%) catalyst required temperatures of at least 700 °C to obtain XRD peaks attributable to carbon nanotubes (CNTs). The CQNs prepared using a Ni/CaO catalyst of various Ni contents showed varying diameters and the remaining catalyst metal particles could still be observed in the samples. Thermogravimetric analysis of the CQNs showed that there were two major weight losses due to the amorphous carbon decomposition (300-400 °C) and oxidation of CNTs (400-600 °C). Raman spectroscopy results showed that the CQNs with the highest graphitization were synthesized using Ni/CaO (10 wt%) at 800 °C with an IG/ID ratio of 1.30. The cyclic voltammetry (CV) of screen-printed carbon electrodes (SPCEs) modified with the CQNs showed that the performance of nanocomposite-modified SPCEs were better than bare SPCEs. When compared to carboxylated multi-walled carbon nanotubes or MWNT-COOH-modified SPCEs, the CQNs synthesized using Ni/CaO (10 wt%) at 800 °C gave higher CV peak currents and comparable electron transfer, making it a good alternative for screen-printed electrode modification.
    Matched MeSH terms: Spectrum Analysis, Raman
  11. Mustapha Kamil Y, Al-Rekabi SH, Yaacob MH, Syahir A, Chee HY, Mahdi MA, et al.
    Sci Rep, 2019 09 17;9(1):13483.
    PMID: 31530893 DOI: 10.1038/s41598-019-49891-7
    The exponential escalation of dengue cases has indeed become a global health crisis. This work elaborates on the development of a biofunctionalized tapered optical fiber (TOF) based sensor with the integration of polyamidoamine (PAMAM) dendrimer for the detection of dengue E protein. The dimension of the TOF generated an evanescent field that was sensitive to any changes in the external medium while the integration of PAMAM promoted more adhesion of bio-recognition molecules; anti-DENV II E protein antibodies; that were complementary to the targeted protein. This in return created more active sites for the absorption of DENV II E proteins onto the tapered region. The resolution and detection limit of the sensor are 19.53 nm/nM and 1 pM, respectively with Kd = 1.02 × 10-10 M.
    Matched MeSH terms: Spectrum Analysis, Raman
  12. Usman MS, Hussein MZ, Kura AU, Fakurazi S, Masarudin MJ, Ahmad Saad FF
    Molecules, 2018 Feb 24;23(2).
    PMID: 29495251 DOI: 10.3390/molecules23020500
    We have synthesized a graphene oxide (GO)-based theranostic nanodelivery system (GOTS) for magnetic resonance imaging (MRI) using naturally occurring protocatechuic acid (PA) as an anticancer agent and gadolinium (III) nitrate hexahydrate (Gd) as the starting material for a contrast agent,. Gold nanoparticles (AuNPs) were subsequently used as second diagnostic agent. The GO nanosheets were first prepared from graphite via the improved Hummer's protocol. The conjugation of the GO and the PA was done via hydrogen bonding and π-π stacking interactions, followed by surface adsorption of the AuNPs through electrostatic interactions. GAGPA is the name given to the nanocomposite obtained from Gd and PA conjugation. However, after coating with AuNPs, the name was modified to GAGPAu. The physicochemical properties of the GAGPA and GAGPAu nanohybrids were studied using various characterization techniques. The results from the analyses confirmed the formation of the GOTS. The powder X-ray diffraction (PXRD) results showed the diffractive patterns for pure GO nanolayers, which changed after subsequent conjugation of the Gd and PA. The AuNPs patterns were also recorded after surface adsorption. Cytotoxicity and magnetic resonance imaging (MRI) contrast tests were also carried out on the developed GOTS. The GAGPAu was significantly cytotoxic to the human liver hepatocellular carcinoma cell line (HepG2) but nontoxic to the standard fibroblast cell line (3T3). The GAGPAu also appeared to possess higher T1 contrast compared to the pure Gd and water reference. The GOTS has good prospects of serving as future theranostic platform for cancer chemotherapy and diagnosis.
    Matched MeSH terms: Spectrum Analysis, Raman
  13. Daood U, Abduljabbar T, Al-Hamoudi N, Akram Z
    J Periodontal Res, 2018 Feb;53(1):123-130.
    PMID: 28940417 DOI: 10.1111/jre.12496
    BACKGROUND AND OBJECTIVE: The aim of the present study was to compare clinical periodontal parameters and to assess the release of C-telopeptides pyridinoline cross-links (ICTP) and C-terminal crosslinked telopeptide (CTX) from gingival collagen of naswar (NW) and non-naswar (control) dippers.

    MATERIAL AND METHODS: Eighty-seven individuals (42 individuals consuming NW and 45 controls) were included. Clinical (plaque index, bleeding on probing, probing depth and clinical attachment loss) and radiographic (marginal bone loss) periodontal parameters were compared among NW and control groups. Gingival specimens were taken from subjects in NW and control groups, assessed for ICTP and CTX levels (using ELISA) and analyzed using micro-Raman spectroscopy. The significance of differences in periodontal parameters between the groups was determined using Kruskal-Wallis and Mann-Whitney U tests. The percent loss of dry mass over exposure time and the rate of release of ICTP and CTX from all groups were compared using the paired t-test to examine the effects of exposure time.

    RESULTS: Clinical and radiographic periodontal parameters were significantly higher in the NW group than the control group (P Raman spectrum, the strongest and sharpest band occurred at 1260 cm-1 amongst NW users. A Raman band at Amide I was observed with slight shifts in wave numbers. The rate of ICTP and CTX release was significantly higher in subjects from the NW group compared with those from the control group (P 

    Matched MeSH terms: Spectrum Analysis, Raman
  14. Azman NZM, Zainal PNS, Alang Ahmad SA
    PLoS One, 2020;15(6):e0234148.
    PMID: 32502185 DOI: 10.1371/journal.pone.0234148
    In this paper, Response Surface Methodology with central composite design (RSM/CCD) was used to optimize a modified electrode for improved electron transfer rate and electrochemical performance. The modification was done on a screen-printed carbon electrode (SPCE) with reduced graphene oxide (ERGO)/calix [4] arene (ERGOC4-SPCE). The properties of the modified electrodes were analyzed via cyclic voltammetry, Raman spectroscopy, and Fourier-Transform Infrared (FT-IR) spectroscopy. Then, different variables were optimized, namely, the concentration of graphene oxide, GO (A), the number of scan cycles of graphene oxide (B), and the deposition time (C). The effect of the optimized variables on the reduction-oxidation peak current response of the potassium ferricyanide redox system was analyzed. By using statistical analysis, it shows a significant effect of the concentration of GO, the deposition time, and the number of scans cycles on the peak current response. The coefficient of determination (R2) value of 0.9987 produced indicated a good fit of the model with experimental finding.
    Matched MeSH terms: Spectrum Analysis, Raman
  15. Manawi Y, Kochkodan V, Mahmoudi E, Johnson DJ, Mohammad AW, Atieh MA
    Sci Rep, 2017 Nov 20;7(1):15831.
    PMID: 29158521 DOI: 10.1038/s41598-017-14735-9
    Novel polyethersulfone (PES) membranes blended with 0.1-3.0 wt. % of Acacia gum (AG) as a pore-former and antifouling agent were fabricated using phase inversion technique. The effect of AG on the pore-size, porosity, surface morphology, surface charge, hydrophilicity, and mechanical properties of PES/AG membranes was studied by scanning electron microscopy (SEM), Raman spectroscopy, contact angle and zeta potential measurements. The antifouling -properties of PES/AG membranes were evaluated using Escherichia coli bacteria and bovine serum albumine (BSA). The use of AG as an additive to PES membranes was found to increase the surface charge, hydrophilicity (by 20%), porosity (by 77%) and permeate flux (by about 130%). Moreover, PES/AG membranes demonstrated higher antifouling and tensile stress (by 31%) when compared to pure PES membranes. It was shown that the prepared PES/AG membranes efficiently removed lead ions from aqueous solutions. Both the sieving mechanism of the membrane and chelation of lead with AG macromolecules incorporated in the membrane matrix contributed to lead removal. The obtained results indicated that AG can be used as a novel pore-former, hydrophilizing and antifouling agent, as well as an enhancer to the mechanical and rejection properties of the PES membranes.
    Matched MeSH terms: Spectrum Analysis, Raman
  16. Teh AA, Ahmad R, Kara M, Rusop M, Awang Z
    J Nanosci Nanotechnol, 2012 Oct;12(10):8201-4.
    PMID: 23421197
    We report the use of a new precursor as active agents to promote the growth of carbon nanotubes (CNT) in methane ambient using a simple thermal chemical vapour deposition method. The agents consist of ammonia and methanol mixed at different ratios and was found to enhance the growth of CNTs. The optimum methanol to ammonia ratio was found to be 8 to 5, whereby longer and denser CNTs were produced compared to other ratios. The result was found otherwise when the experiment was done solely in methane ambient. In addition, CNT growth on substrates coated with double layer Ni catalyst was improved in terms of quality and density compared to a single coated substrates. This finding is supported by Raman spectrometry analysis.
    Matched MeSH terms: Spectrum Analysis, Raman
  17. Sadri R, Hosseini M, Kazi SN, Bagheri S, Zubir N, Solangi KH, et al.
    J Colloid Interface Sci, 2017 Oct 15;504:115-123.
    PMID: 28531649 DOI: 10.1016/j.jcis.2017.03.051
    In this study, we propose an innovative, bio-based, environmentally friendly approach for the covalent functionalization of multi-walled carbon nanotubes using clove buds. This approach is innovative because we do not use toxic and hazardous acids which are typically used in common carbon nanomaterial functionalization procedures. The MWCNTs are functionalized in one pot using a free radical grafting reaction. The clove-functionalized MWCNTs (CMWCNTs) are then dispersed in distilled water (DI water), producing a highly stable CMWCNT aqueous suspension. The CMWCNTs are characterized using Raman spectroscopy, X-ray photoelectron spectroscopy and transmission electron microscopy. The electrostatic interactions between the CMWCNT colloidal particles in DI water are verified via zeta potential measurements. UV-vis spectroscopy is also used to examine the stability of the CMWCNTs in the base fluid. The thermo-physical properties of the CMWCNT nano-fluids are examined experimentally and indeed, this nano-fluid shows remarkably improved thermo-physical properties, indicating its superb potential for various thermal applications.
    Matched MeSH terms: Spectrum Analysis, Raman
  18. Edueng K, Mahlin D, Larsson P, Bergström CAS
    J Control Release, 2017 06 28;256:193-202.
    PMID: 28412224 DOI: 10.1016/j.jconrel.2017.04.015
    We developed a step-by-step experimental protocol using differential scanning calorimetry (DSC), dynamic vapour sorption (DVS), polarized light microscopy (PLM) and a small-scale dissolution apparatus (μDISS Profiler) to investigate the mechanism (solid-to-solid or solution-mediated) by which crystallization of amorphous drugs occurs upon dissolution. This protocol then guided how to stabilize the amorphous formulation. Indapamide, metolazone, glibenclamide and glipizide were selected as model drugs and HPMC (Pharmacoat 606) and PVP (K30) as stabilizing polymers. Spray-dried amorphous indapamide, metolazone and glibenclamide crystallized via solution-mediated nucleation while glipizide suffered from solid-to-solid crystallization. The addition of 0.001%-0.01% (w/v) HPMC into the dissolution medium successfully prevented the crystallization of supersaturated solutions of indapamide and metolazone whereas it only reduced the crystallization rate for glibenclamide. Amorphous solid dispersion (ASD) formulation of glipizide and PVP K30, at a ratio of 50:50% (w/w) reduced but did not completely eliminate the solid-to-solid crystallization of glipizide even though the overall dissolution rate was enhanced both in the absence and presence of HPMC. Raman spectroscopy indicated the formation of a glipizide polymorph in the dissolution medium with higher solubility than the stable polymorph. As a complementary technique, molecular dynamics (MD) simulations of indapamide and glibenclamide with HPMC was performed. It was revealed that hydrogen bonding patterns of the two drugs with HPMC differed significantly, suggesting that hydrogen bonding may play a role in the greater stabilizing effect on supersaturation of indapamide, compared to glibenclamide.
    Matched MeSH terms: Spectrum Analysis, Raman
  19. Edueng K, Mahlin D, Gråsjö J, Nylander O, Thakrani M, Bergström CAS
    Molecules, 2019 Jul 27;24(15).
    PMID: 31357587 DOI: 10.3390/molecules24152731
    This study explores the effect of physical aging and/or crystallization on the supersaturation potential and crystallization kinetics of amorphous active pharmaceutical ingredients (APIs). Spray-dried, fully amorphous indapamide, metolazone, glibenclamide, hydrocortisone, hydrochlorothiazide, ketoconazole, and sulfathiazole were used as model APIs. The parameters used to assess the supersaturation potential and crystallization kinetics were the maximum supersaturation concentration (Cmax,app), the area under the curve (AUC), and the crystallization rate constant (k). These were compared for freshly spray-dried and aged/crystallized samples. Aged samples were stored at 75% relative humidity for 168 days (6 months) or until they were completely crystallized, whichever came first. The solid-state changes were monitored with differential scanning calorimetry, Raman spectroscopy, and powder X-ray diffraction. Supersaturation potential and crystallization kinetics were investigated using a tenfold supersaturation ratio compared to the thermodynamic solubility using the µDISS Profiler. The physically aged indapamide and metolazone and the minimally crystallized glibenclamide and hydrocortisone did not show significant differences in their Cmax,app and AUC when compared to the freshly spray-dried samples. Ketoconazole, with a crystalline content of 23%, reduced its Cmax,app and AUC by 50%, with Cmax,app being the same as the crystalline solubility. The AUC of aged metolazone, one of the two compounds that remained completely amorphous after storage, significantly improved as the crystallization kinetics significantly decreased. Glibenclamide improved the most in its supersaturation potential from amorphization. The study also revealed that, besides solid-state crystallization during storage, crystallization during dissolution and its corresponding pathway may significantly compromise the supersaturation potential of fully amorphous APIs.
    Matched MeSH terms: Spectrum Analysis, Raman
  20. Zen DI, Saidin N, Damanhuri SS, Harun SW, Ahmad H, Ismail MA, et al.
    Appl Opt, 2013 Feb 20;52(6):1226-9.
    PMID: 23434993 DOI: 10.1364/AO.52.001226
    We demonstrate mode locking of a thulium-bismuth codoped fiber laser (TBFL) operating at 1901.6 nm, using a graphene-based saturable absorber (SA). In this work, a single layer graphene is mechanically exfoliated using the scotch tape method and directly transferred onto the surface of a fiber pigtail to fabricate the SA. The obtained Raman spectrum characteristic indicates that the graphene on the core surface has a single layer. At 1552 nm pump power of 869 mW, the mode-locked TBFL self starts to generate an optical pulse train with a repetition rate of 16.7 MHz and pulse width of 0.37 ps. This is a simple, low-cost, stable, and convenient laser oscillator for applications where eye-safe and low-photon-energy light sources are required, such as sensing and biomedical diagnostics.
    Matched MeSH terms: Spectrum Analysis, Raman/methods
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