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Pyrolytic conversion of human hair to fuel: performance evaluation and kinetic modelling

Krishnakumar P, Sundaramurthy S, Baredar P, Suresh A, Khan MA, Sharma G, et al.

Environ Sci Pollut Res Int, 2023 Dec;30(60):125104-125116.
PMID: 37099105 DOI: 10.1007/s11356-023-26991-6

There are several environmental and human health impacts if human hair waste is not adequately disposed of. In this study, pyrolysis of discarded human hair was carried out. This research focused on the pyrolysis of discarded human hair under controlled environmental conditions. The effects of the mass of discarded human hair and temperature on bio-oil yield were studied. The proximate and ultimate analyses and calorific values of disposed of human hair, bio-oil, and biochar were determined. Further, chemical compounds of bio-oil were analyzed using a gas chromatograph and a mass spectrometer. Finally, the kinetic modeling and behavior of the pyrolysis process were characterized through FT-IR spectroscopy and thermal analysis. Based on the optimized mass of disposed of human hair, 250 g had a better bio-oil yield of 97% in the temperature range of 210-300 °C. The different parameters of bio-oil were: pH (2.87), specific gravity (1.17), moisture content (19%), heating value (19.34 MJ/kg), and viscosity (50 CP). C (56.4%), H (6.1%), N (0.16%), S (0.01%), O (38.4%), and Ash (0.1%) were discovered to be the elemental chemical composition of bio-oil (on a dry basis). During breakdown, the release of different compounds like hydrocarbons, aldehydes, ketones, acids, and alcohols takes place. According to the GC-MS results, several amino acids were discovered in the bio-oil, 12 abundant in the discarded human hair. The FTIR and thermal analysis found different concluding temperatures and wave numbers for functional groups. Two main stages are partially separated at about 305 °C, with maximum degradation rates at about 293 oC and 400-4140 °C, respectively. The mass loss was 30% at 293 0C and 82% at temperatures above 293 0C. When the temperature reached 4100C, the entire bio-oil from discarded human hair was distilled or thermally decomposed.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared
Fulltext Characterization, Synthesis, and Biological Activities of Silver Nanoparticles Produced via Green Synthesis Method Using Thymus Vulgaris Aqueous Extract

Ejaz U, Afzal M, Mazhar M, Riaz M, Ahmed N, Rizg WY, et al.

Int J Nanomedicine, 2024;19:453-469.
PMID: 38250190 DOI: 10.2147/IJN.S446017

INTRODUCTION: Silver nanoparticles (AgNPs) have been found to exhibit unique properties which show their potential to be used in various therapies. Green synthesis of AgNPs has been progressively gaining acceptance due to its cost-effectiveness and energy-efficient nature.
OBJECTIVE: In the current study, aqueous extract of Thymus vulgaris (T. vulgaris) was used to synthesize the AgNPs using green synthesis techniques followed by checking the effectiveness and various biological activities of these AgNPs.
METHODS: At first, the plant samples were proceeded for extraction of aqueous extracts followed by chromatography studies to measure the phenolics and flavonoids. The synthesis and characterization of AgNPs were done using green synthesis techniques and were confirmed using Fourier transform infra-red (FT-IR) spectroscopy, UV-visible spectroscopy, scanning electron microscope (SEM), zeta potential, zeta sizer and X-Ray diffraction (XRD) analysis. After confirmation of synthesized AgNPs, various biological activities were checked.
RESULTS: The chromatography analysis detected nine compounds accounting for 100% of the total amount of plant constituents. The FT-IR, UV-vis spectra, SEM, zeta potential, zeta sizer and XRD analysis confirmed the synthesis of AgNPs and the variety of chemical components present on the surface of synthesized AgNPs in the plant extract. The antioxidant activity of AgNPs showed 92% inhibition at the concentration of at 1000 µg/mL. A greater inhibitory effect in anti-diabetic analysis was observed with synthesized AgNPs as compared to the standard AgNPs. The hemolytic activity was low, but despite low concentrations of hemolysis activity, AgNPs proved not to be toxic or biocompatible. The anti-inflammatory activity of AgNPs was observed by in-vitro and in-vivo approaches in range at various concentrations, while maximum inhibition occurs at 1000 µg (77.31%).
CONCLUSION: Our data showed that the potential biological activities of the bioactive constituents of T. vulgaris can be enhanced through green synthesis of AgNPs from T. vulgaris aqueous extracts. In addition, the current study depicted that AgNPs have good potential to cure different ailments as biogenic nano-medicine.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared
Microencapsulation of Citrus Grandis Peel Oil Using Interfacial Precipitation Chemistry Technique for Repellent Application

Misni N, Mohamed Nor Z, Ahmad R

Iran J Pharm Res, 2019;18(1):198-209.
PMID: 31089355

Essential oil of Citrus family plant is known to have repellent effect against mosquito. Unfortunately, due to its high volatility effect, its repellency effect was compromised. The incorporation of essential oil in a microencapsulation formulation has been shown to help improve the stability and potency of the repellent. In this study, Citrus grandis peel oil (CGPO) was encapsulated by using the interfacial precipitation chemistry technique. The microencapsulated CGPO was then formulated into lotion form to produce topical repellent formulation. This study includes the characterization of microcapsules with regards to the morphology, size distribution, zeta potential, Fourier Transmission Infrared spectrophotometer (FTIR), and Thermogravity analysis (TGA). The effectiveness of the microencapsulated CGPO-lotion formulation against mosquitoes was evaluated in the laboratory setting. Results indicated that CGPO have been successfully encapsulated with 6.5 µm in diameter and zeta potential values, -47.9 mV. The FTIR analysis spectrum indicated the presence of interaction between the wall materials in microcapsules. The TGA analysis demonstrated that microencapsulation improved the thermal stability of CGPO. Repellency assay revealed that microencapsulated CGPO- based formulation possessed excellent effect compared with pure CGPO. In conclusion, CGPO was successfully encapsulated and the microencapsulation aid to improve the repellency effect of CGPO against mosquito bites.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared
Fulltext Preparation and characterisation of ciprofloxacin-loaded silver nanoparticles for drug delivery

Hussein-Al-Ali SH, Abudoleh SM, Abualassal QIA, Abudayeh Z, Aldalahmah Y, Hussein MZ

IET Nanobiotechnol, 2022 May;16(3):92-101.
PMID: 35332980 DOI: 10.1049/nbt2.12081

Silver nanoparticles (AgNPs) have shown potential applications in drug delivery. In this study, the AgNPs was prepared from silver nitrate in the presence of alginate as a capping agent. The ciprofloxacin (Cipro) was loaded on the surface of AgNPs to produce Cipro-AgNPs nanocomposite. The characteristics of the Cipro-AgNPs nanocomposite were studied by X-ray diffraction (XRD), UV-Vis, transmission electron microscopy (TEM), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), Fourier-transform infra-red analysis (FT-IR) and zeta potential analyses. The XRD of AgNPs and Cipro-AgNPs nanocomposite data showed that both have a crystalline structure in nature. The FT-IR data indicate that the AgNPs have been wrapped by the alginate and loaded with the Cipro drug. The TEM image showed that the Cipro-AgNPs nanocomposites have an average size of 96 nm with a spherical shape. The SEM image for AgNPs and Cipro-AgNPs nanocomposites confirmed the needle-lumpy shape. The zeta potential for Cipro-AgNPs nanocomposites exhibited a positive charge with a value of 6.5 mV. The TGA for Cipro-AgNPs nanocomposites showed loss of 79.7% in total mass compared to 57.6% for AgNPs which is due to the Cipro loaded in the AgNPs. The release of Cipro from Cipro-AgNPs nanocomposites showed slow release properties which reached 98% release within 750 min, and followed the Hixson-Crowell kinetic model. In addition, the toxicity of AgNPs and Cipro-AgNPs nanocomposites was evaluated using normal (3T3) cell line. The present work suggests that Cipro-AgNPs are suitable for drug delivery.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared
Quantifying carbon pool in ex-mining lake-converted constructed wetlands of Paya Indah Wetlands, Selangor, Malaysia

Jamion NA, Lee KE, Mokhtar M, Goh TL

Environ Sci Pollut Res Int, 2024 Mar;31(11):16291-16308.
PMID: 38315340 DOI: 10.1007/s11356-024-32140-4

Ex-mining lake-converted constructed wetlands play a significant role in the carbon cycle, offering a great potential to sequester carbon and mitigate climate change and global warming. Investigating the quantity of carbon storage capacity of ex-mining lake-converted constructed wetlands provides information and justification for restoration and conservation efforts. The present study aims to quantify the carbon pool of the ex-mining lake-converted constructed wetlands and characterise the physicochemical properties of the soil and sediment. Pearson's correlation and a one-way ANOVA were performed to compare the different sampling stations at Paya Indah Wetland, Selangor, Malaysia. An analysis of 23 years of ex-mining lake-converted constructed wetlands of Paya Indah Wetlands, Selangor, Malaysia, revealed that the estimated total carbon pool in soil and sediment accumulated to 1553.11 Mg C ha-1 (equivalent to 5700 Mg CO2 ha-1), which translates to an annual carbon sink capacity of around 67.5 Mg C ha-1 year-1. The characterisation showed that the texture of all soil samples was dominated by silt, whereas sediments exhibited texture heterogeneity. Although the pH of the soil and sediment was both acidic, the bulk density was still optimal for plant growth and did not affect root growth. FT-IR and WDXRF results supported that besides the accumulation and degradation of organic substances, which increase the soil and sediment carbon content, mineral carbonation is a mechanism by which soil and sediment can store carbon. Therefore, this study indicates that the ex-mining lake-converted constructed wetlands of Paya Indah Wetlands, Selangor, Malaysia have a significant carbon storage potential.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared
Isolation and characterization of cellulose nanofibers from Agave gigantea by chemical-mechanical treatment

Syafri E, Jamaluddin, Sari NH, Mahardika M, Amanda P, Ilyas RA

Int J Biol Macromol, 2022 Mar 01;200:25-33.
PMID: 34971644 DOI: 10.1016/j.ijbiomac.2021.12.111

Nanocellulose is a renewable and biocompatible nanomaterial that evokes much interest because of its versatility in various applications. This study reports the production of nanocellulose from Agave gigantea (AG) fiber using the chemical-ultrafine grinding treatment. Chemical treatment (alkalization and bleaching) removed non-cellulose components (hemicellulose and lignin), while ultrafine grinding reduced the size of cellulose microfibrils into nanocellulose. From the observation of Transmission Electron Microscopy, the average diameter of nanocellulose was 4.07 nm. The effect of chemical-ultrafine grinding on the morphology and properties of AG fiber was identified using chemical composition, Scanning Electron Microscopy, X-ray Diffraction, Fourier Transform Infrared, and Thermogravimetric Analysis. The bleaching treatment increased the crystal index by 48.3% compared to raw AG fiber, along with an increase in the cellulose content of 20.4%. The ultrafine grinding process caused a decrease in the crystal content of the AG fiber. The crystal index affected the thermal stability of the AG fiber. The TGA results showed that AG fiber treated with bleaching showed the highest thermal stability compared to AG fiber without treatment. The FTIR analysis showed that the presence of CH vibrations from the ether in the fiber. After chemical treatment, the peaks at 1605 and 1243 cm-1 disappeared, indicating the loss of lignin and hemicellulose functional groups in AG fiber. As a result, nanocellulose derived from AG fiber can be applied as reinforcement in environmentally friendly polymer biocomposites.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared
Thermal properties analysis and thermal cycling of HITEC molten salt with h-BN nanoparticles for CSP thermal energy storage applications

Suraparaju SK, Aljaerani HA, Samykano M, Kadirgama K, Noor MM, Natarajan SK

Environ Sci Pollut Res Int, 2024 Aug;31(38):50166-50178.
PMID: 38625473 DOI: 10.1007/s11356-024-33151-x

Molten salts are the operational fluid for most concentrated solar power (CSP) systems, which has attracted more attention among the scientific community due to the augmentation of their properties with the doping of nanoparticles. Hexagonal boron nitride (h-BN) nanoparticles were dispersed in HITEC molten salt to create a novel nanofluid and evaluate the h-BN nanoparticles' influence on HITEC thermophysical properties. The influence of nanoparticle concentration (0.1, 0.5, and 1wt.%) of h-BN and HITEC was studied in this research. HITEC and nano-enhanced HITEC molten salt (NEHMS) were characterized using energy-dispersive X-ray spectroscopy (EDX), field emission scanning electron microscopy (FESEM), and Fourier transform infrared spectroscopy (FT-IR). Specific heat capacity, latent heat, and melting temperature were assessed using differential scanning calorimetry (DSC). The maximum working temperature was evaluated with thermogravimetric analysis (TGA). The ideal nanoparticle concentration is 0.1 wt.% h-BN, which results in a 27% increase in heat capacity, a 72% increase in latent heat, and a 7% enhancement in thermal stability. The thermal cycling stability test proved the stability of the enhanced thermophysical properties. The material characterization revealed that the samples with improved thermophysical properties have a homogeneous dispersion of nanoparticles with minor nanoparticle agglomeration. The system advisor model (SAM) simulation comparison of the optimum sample with solar salt and HITEC salt revealed that using the optimum sample increases CSP plant efficiency by 0.4% and reduces power costs by 0.13¢/kWh.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared
Quantitative characterization of chitosan in the skin by Fourier-transform infrared spectroscopic imaging and ninhydrin assay: application in transdermal sciences

Nawaz A, Wong TW

J Microsc, 2016 07;263(1):34-42.
PMID: 26695532 DOI: 10.1111/jmi.12371

The chitosan has been used as the primary excipient in transdermal particulate dosage form design. Its distribution pattern across the epidermis and dermis is not easily accessible through chemical assay and limited to radiolabelled molecules via quantitative autoradiography. This study explored Fourier-transform infrared spectroscopy imaging technique with built-in microscope as the means to examine chitosan molecular distribution over epidermis and dermis with the aid of histology operation. Fourier-transform infrared spectroscopy skin imaging was conducted using chitosan of varying molecular weights, deacetylation degrees, particle sizes and zeta potentials, obtained via microwave ligation of polymer chains at solution state. Both skin permeation and retention characteristics of chitosan increased with the use of smaller chitosan molecules with reduced acetyl content and size, and increased positive charge density. The ratio of epidermal to dermal chitosan content decreased with the use of these chitosan molecules as their accumulation in dermis (3.90% to 18.22%) was raised to a greater extent than epidermis (0.62% to 1.92%). A larger dermal chitosan accumulation nonetheless did not promote the transdermal polymer passage more than the epidermal chitosan. A small increase in epidermal chitosan content apparently could fluidize the stratum corneum and was more essential to dictate molecular permeation into dermis and systemic circulation. The histology technique aided Fourier-transform infrared spectroscopy imaging approach introduces a new dimension to the mechanistic aspect of chitosan in transdermal delivery.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods*
Fulltext Development and characterization of poly(1-vinylpyrrolidone-co-vinyl acetate) copolymer based polymer electrolytes

Sa'adun NN, Subramaniam R, Kasi R

ScientificWorldJournal, 2014;2014:254215.
PMID: 25431781 DOI: 10.1155/2014/254215

Gel polymer electrolytes (GPEs) are developed using poly(1-vinylpyrrolidone-co-vinyl acetate) [P(VP-co-VAc)] as the host polymer, lithium bis(trifluoromethane) sulfonimide [LiTFSI] as the lithium salt and ionic liquid, and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide [EMImTFSI] by using solution casting technique. The effect of ionic liquid on ionic conductivity is studied and the optimum ionic conductivity at room temperature is found to be 2.14 × 10(-6) S cm(-1) for sample containing 25 wt% of EMImTFSI. The temperature dependence of ionic conductivity from 303 K to 353 K exhibits Arrhenius plot behaviour. The thermal stability of the polymer electrolyte system is studied by using thermogravimetric analysis (TGA) while the structural and morphological properties of the polymer electrolyte is studied by using Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction analysis (XRD), respectively.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods
Investigation of interaction studies of cefpirome with ACE-inhibitors in various buffers

Nawaz M, Arayne MS, Sultana N, Abbas HF

Spectrochim Acta A Mol Biomol Spectrosc, 2015 Feb 25;137:1050-4.
PMID: 25300038 DOI: 10.1016/j.saa.2014.08.152

This work describes a RP-HPLC method for the determination and interaction studies of cefpirome with ACE-inhibitors (captopril, enalapril and lisinopril) in various buffers. The separation and interaction of cefpirome with ACE-inhibitors was achieved on a Purospher Star, C18 (5 μm, 250×4.6 mm) column. Mobile phase consisted of methanol: water (80:20, v/v, pH 3.3); however, for the separation of lisinopril, it was modified to methanol-water (40:60, v/v, pH 3.3) and pumped at a flow rate of 1 mL min(-1). In all cases, UV detection was performed at 225 nm. Interactions were carried out in physiological pH i.e., pH 1 (simulated gastric juice), 4 (simulated full stomach), 7.4 (blood pH) and 9 (simulated GI), drug contents were analyzed by reverse phase high performance liquid chromatography. Method was found linear in the concentration range of 1.0-50.0 μg mL(-1) with correlation coefficient (r(2)) of 0.999. Precision (RSD%) was less than 2.0%, indicating good precision of the method and accuracy was 98.0-100.0%. Furthermore, cefpirome-ACE-inhibitors' complexes were also synthesized and results were elucidated on the basis of FT-IR, and (1)H NMR. The interaction results show that these interactions are pH dependent and for the co-administration of cefpirome and ACE-inhibitors, a proper interval should be given.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods
Two-dimensional correlation infrared spectroscopy applied to analyzing and identifying the extracts of Baeckea frutescens medicinal materials

Adib AM, Jamaludin F, Kiong LS, Hashim N, Abdullah Z

J Pharm Biomed Anal, 2014 Aug 5;96:104-10.
PMID: 24727283 DOI: 10.1016/j.jpba.2014.03.022

Baeckea frutescens or locally known as Cucur atap is used as antibacterial, antidysentery, antipyretic and diuretic agent. In Malaysia and Indonesia, they are used as an ingredient of the traditional medicine given to mothers during confinement. A three-steps infra-red (IR) macro-fingerprinting method combining conventional IR spectra, and the secondary derivative spectra with two dimensional infrared correlation spectroscopy (2D-IR) have been proved to be effective methods to examine a complicated mixture such as herbal medicines. This study investigated the feasibility of employing multi-steps IR spectroscopy in order to study the main constituents of B. frutescens and its different extracts (extracted by chloroform, ethyl acetate, methanol and aqueous in turn). The findings indicated that FT-IR and 2D-IR can provide many holistic variation rules of chemical constituents. The structural information of the samples indicated that B. frutescens and its extracts contain a large amount of flavonoids, since some characteristic absorption peaks of flavonoids, such as ∼1600cm(-1), ∼1500cm(-1), ∼1450cm(-1), and ∼1270cm(-1) can be observed. The macroscopical fingerprint characters of FT-IR and 2D-IR spectra can not only provide the information of main chemical constituents in medicinal materials and their different extracts, but also compare the components differences among the similar samples. In conclusion, the multi-steps IR macro-fingerprint method is rapid, effective, visual and accurate for pharmaceutical research.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods*
Conductivity and FTIR studies on PEO-LiX [X: CF3SO3(-), SO4(2-)] polymer electrolytes

Ramesh S, Yuen TF, Shen CJ

Spectrochim Acta A Mol Biomol Spectrosc, 2008 Feb;69(2):670-5.
PMID: 17600757

Polymer electrolytes based on poly(ethylene oxide)-lithium triflate (PEO-LiCF3SO3) and poly(ethylene oxide)-lithium sulphate (PEO-Li2S4) were prepared by using solution casting method. Measurements of conductivity and dielectric were carried out on these films as a function of frequency at various temperatures. It was observed that PEO-LiCF3SO3 polymer electrolytes have higher conductivity. The interaction between PEO and Li salts were studied by Fourier transform infrared (FTIR).

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods*
Fulltext Synthesis, molecular structure and spectroscopic investigations of novel fluorinated spiro heterocycles

Islam MS, Al-Majid AM, Barakat A, Soliman SM, Ghabbour HA, Quah CK, et al.

Molecules, 2015 May 07;20(5):8223-41.
PMID: 25961163 DOI: 10.3390/molecules20058223

This paper describes an efficient and regioselective method for the synthesis of novel fluorinated spiro-heterocycles in excellent yield by cascade [5+1] double Michael addition reactions. The compounds 7,11-bis(4-fluorophenyl)-2,4-dimethyl- 2,4-diazaspiro[5.5] undecane-1,3,5,9-tetraone (3a) and 2,4-dimethyl-7,11-bis (4-(trifluoromethyl)phenyl)-2,4-diazaspiro[5.5]undecane-1,3,5,9-tetraone (3b) were characterized by single-crystal X-ray diffraction, FT-IR and NMR techniques. The optimized geometrical parameters, infrared vibrational frequencies and NMR chemical shifts of the studied compounds have also been calculated using the density functional theory (DFT) method, using Becke-3-Lee-Yang-Parr functional and the 6-311G(d,p) basis set. There is good agreement between the experimentally determined structural parameters, vibrational frequencies and NMR chemical shifts of the studied compounds and those predicted theoretically. The calculated natural atomic charges using NBO method showed higher polarity of 3a compared to 3b.The calculated electronic spectra are also discussed based on the TD-DFT calculations.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods
Alteration of the bone tissue material properties in type 1 diabetes mellitus: A Fourier transform infrared microspectroscopy study

Mieczkowska A, Mansur SA, Irwin N, Flatt PR, Chappard D, Mabilleau G

Bone, 2015 Jul;76:31-9.
PMID: 25813583 DOI: 10.1016/j.bone.2015.03.010

Type 1 diabetes mellitus (T1DM) is a severe disorder characterized by hyperglycemia and hypoinsulinemia. A higher occurrence of bone fractures has been reported in T1DM, and although bone mineral density is reduced in this disorder, it is also thought that bone quality may be altered in this chronic pathology. Vibrational microscopies such as Fourier transform infrared microspectroscopy (FTIRM) represent an interesting approach to study bone quality as they allow investigation of the collagen and mineral compartment of the extracellular matrix in a specific bone location. However, as spectral feature arising from the mineral may overlap with those of the organic component, the demineralization of bone sections should be performed for a full investigation of the organic matrix. The aims of the present study were to (i) develop a new approach, based on the demineralization of thin bone tissue section to allow a better characterization of the bone organic component by FTIRM, (ii) to validate collagen glycation and collagen integrity in bone tissue and (iii) to better understand what alterations of tissue material properties in newly forming bone occur in T1DM. The streptozotocin-injected mouse (150 mg/kg body weight, injected at 8 weeks old) was used as T1DM model. Animals were randomly allocated to control (n = 8) or diabetic (n = 10) groups and were sacrificed 4 weeks post-STZ injection. Bones were collected at necropsy, embedded in polymethylmethacrylate and sectioned prior to examination by FTIRM. FTIRM collagen parameters were collagen maturity (area ratio between 1660 and 1690 cm(-1) subbands), collagen glycation (area ratio between the 1032 cm(-1) subband and amide I) and collagen integrity (area ratio between the 1338 cm(-1) subband and amide II). No significant differences in the mineral compartment of the bone matrix could be observed between controls and STZ-injected animals. On the other hand, as compared with controls, STZ-injected animals presented with significant higher value for collagen maturity (17%, p = 0.0048) and collagen glycation (99%, p = 0.0121), while collagen integrity was significantly lower by 170% (p = 0.0121). This study demonstrated the profound effect of early T1DM on the organic compartment of the bone matrix in newly forming bone. Further studies in humans are required to ascertain whether T1DM also lead to similar effect on the quality of the bone matrix.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods*
Molecular Dynamics and Physical Stability of Pharmaceutical Co-amorphous Systems: Correlation Between Structural Relaxation Times Measured by Kohlrausch-Williams-Watts With the Width of the Glass Transition Temperature (ΔTg) and the Onset of Crystallization

Chieng N, Teo X, Cheah MH, Choo ML, Chung J, Hew TK, et al.

J Pharm Sci, 2019 12;108(12):3848-3858.
PMID: 31542436 DOI: 10.1016/j.xphs.2019.09.013

The study aims to characterize the structural relaxation times of quench-cooled co-amorphous systems using Kohlrausch-Williams-Watts (KWW) and to correlate the relaxation data with the onset of crystallization. Comparison was also made between the relaxation times obtained by KWW and the width of glass transition temperature (ΔTg) methods (simple and quick). Differential scanning calorimetry, Fourier-transformed infrared spectroscopy, and polarized light microscopy were used to characterize the systems. Results showed that co-amorphous systems yielded a single Tg and ΔCp, suggesting the binary mixtures exist as a single amorphous phase. A narrow step change at Tg indicates the systems were fragile glasses. In co-amorphous nap-indo and para-indo, experimental Tgs were in good agreement with the predicted Tg. However, the Tg of co-amorphous nap-cim and indo-cim were 20°C higher than the predicted Tg, possibly due to stronger molecular interactions. Structural relaxation times below the experimental Tg were successfully characterized using the KWW and ΔTg methods. The comparison plot showed that KWW data are directly proportional to the ½ power of ΔTg data, after adjusting for a small offset. A moderate positive correlation was observed between the onset of crystallization and the KWW data. Structural relaxation times may be useful predictor of physical stability of co-amorphous systems.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods
Comparative study between Pap smear cytology and FTIR spectroscopy: a new tool for screening for cervical cancer

El-Tawil SG, Adnan R, Muhamed ZN, Othman NH

Pathology, 2008 Oct;40(6):600-3.
PMID: 18752127 DOI: 10.1080/00313020802320622

AIMS: To evaluate Fourier transform infrared (FTIR) spectroscopy as new tool for screening of cervical cancer in comparison with cervical cytology.
METHODS: A total of 800 cervical scrapings were taken by cytobrush and placed in ThinPrep medium. The samples were dried over infrared transparent matrix. Beams of infrared light were directed at the dried samples at frequency of 4000 to 400 cm(-1). The absorption data were produced using a Spectrum BX II FTIR spectrometer. Data were compared with the reference absorption data of known samples using FTIR spectroscopy software. FTIR spectroscopy was compared with cytology (gold standard).
RESULTS: FTIR spectroscopy could differentiate normal from abnormal cervical cells in the samples examined. The sensitivity was 85%, specificity 91%, positive predictive value 19.5% and negative predictive value of 99.5%.
CONCLUSION: This study suggests that FTIR spectroscopy could be used as an alternative method for screening for cervical cancer.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared*
Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy as an Analytical Method to Investigate the Secondary Structure of a Model Protein Embedded in Solid Lipid Matrices

Zeeshan F, Tabbassum M, Jorgensen L, Medlicott NJ

Appl Spectrosc, 2018 Feb;72(2):268-279.
PMID: 29022355 DOI: 10.1177/0003702817739908

Protein drugs may encounter conformational perturbations during the formulation processing of lipid-based solid dosage forms. In aqueous protein solutions, attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy can investigate these conformational changes following the subtraction of spectral interference of solvent with protein amide I bands. However, in solid dosage forms, the possible spectral contribution of lipid carriers to protein amide I band may be an obstacle to determine conformational alterations. The objective of this study was to develop an ATR FT-IR spectroscopic method for the analysis of protein secondary structure embedded in solid lipid matrices. Bovine serum albumin (BSA) was chosen as a model protein, while Precirol AT05 (glycerol palmitostearate, melting point 58 ℃) was employed as the model lipid matrix. Bovine serum albumin was incorporated into lipid using physical mixing, melting and mixing, or wet granulation mixing methods. Attenuated total reflection FT-IR spectroscopy and size exclusion chromatography (SEC) were performed for the analysis of BSA secondary structure and its dissolution in aqueous media, respectively. The results showed significant interference of Precirol ATO5 with BSA amide I band which was subtracted up to 90% w/w lipid content to analyze BSA secondary structure. In addition, ATR FT-IR spectroscopy also detected thermally denatured BSA solid alone and in the presence of lipid matrix indicating its suitability for the detection of denatured protein solids in lipid matrices. Despite being in the solid state, conformational changes occurred to BSA upon incorporation into solid lipid matrices. However, the extent of these conformational alterations was found to be dependent on the mixing method employed as indicated by area overlap calculations. For instance, the melting and mixing method imparted negligible effect on BSA secondary structure, whereas the wet granulation mixing method promoted more changes. Size exclusion chromatography analysis depicted the complete dissolution of BSA in the aqueous media employed in the wet granulation method. In conclusion, an ATR FT-IR spectroscopic method was successfully developed to investigate BSA secondary structure in solid lipid matrices following the subtraction of lipid spectral interference. The ATR FT-IR spectroscopy could further be applied to investigate the secondary structure perturbations of therapeutic proteins during their formulation development.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods*
Fulltext Automated cervical precancerous cells screening system based on Fourier transform infrared spectroscopy features

Jusman Y, Mat Isa NA, Ng SC, Hasikin K, Abu Osman NA

J Biomed Opt, 2016 07 01;21(7):75005.
PMID: 27403606 DOI: 10.1117/1.JBO.21.7.075005

Fourier transform infrared (FTIR) spectroscopy technique can detect the abnormality of a cervical cell that occurs before the morphological change could be observed under the light microscope as employed in conventional techniques. This paper presents developed features extraction for an automated screening system for cervical precancerous cell based on the FTIR spectroscopy as a second opinion to pathologists. The automated system generally consists of the developed features extraction and classification stages. Signal processing techniques are used in the features extraction stage. Then, discriminant analysis and principal component analysis are employed to select dominant features for the classification process. The datasets of the cervical precancerous cells obtained from the feature selection process are classified using a hybrid multilayered perceptron network. The proposed system achieved 92% accuracy.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods*
Fulltext Comprehensive Review on Application of FTIR Spectroscopy Coupled with Chemometrics for Authentication Analysis of Fats and Oils in the Food Products

Rohman A, Ghazali MAB, Windarsih A, Irnawati, Riyanto S, Yusof FM, et al.

Molecules, 2020 Nov 23;25(22).
PMID: 33238638 DOI: 10.3390/molecules25225485

Currently, the authentication analysis of edible fats and oils is an emerging issue not only by producers but also by food industries, regulators, and consumers. The adulteration of high quality and expensive edible fats and oils as well as food products containing fats and oils with lower ones are typically motivated by economic reasons. Some analytical methods have been used for authentication analysis of food products, but some of them are complex in sampling preparation and involving sophisticated instruments. Therefore, simple and reliable methods are proposed and developed for these authentication purposes. This review highlighted the comprehensive reports on the application of infrared spectroscopy combined with chemometrics for authentication of fats and oils. New findings of this review included (1) FTIR spectroscopy combined with chemometrics, which has been used to authenticate fats and oils; (2) due to as fingerprint analytical tools, FTIR spectra have emerged as the most reported analytical techniques applied for authentication analysis of fats and oils; (3) the use of chemometrics as analytical data treatment is a must to extract the information from FTIR spectra to be understandable data. Next, the combination of FTIR spectroscopy with chemometrics must be proposed, developed, and standardized for authentication and assuring the quality of fats and oils.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared*
Fulltext Sensitive Detection of Dengue Virus Type 2 E-Proteins Signals Using Self-Assembled Monolayers/Reduced Graphene Oxide-PAMAM Dendrimer Thin Film-SPR Optical Sensor

Omar NAS, Fen YW, Abdullah J, Mustapha Kamil Y, Daniyal WMEMM, Sadrolhosseini AR, et al.

Sci Rep, 2020 02 11;10(1):2374.
PMID: 32047209 DOI: 10.1038/s41598-020-59388-3

In this work, sensitive detection of dengue virus type 2 E-proteins (DENV-2 E-proteins) was performed in the range of 0.08 pM to 0.5 pM. The successful DENV detection at very low concentration is a matter of concern for targeting the early detection after the onset of dengue symptoms. Here, we developed a SPR sensor based on self-assembled monolayer/reduced graphene oxide-polyamidoamine dendrimer (SAM/NH2rGO/PAMAM) thin film to detect DENV-2 E-proteins. Surface characterizations involving X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) confirms the incorporation of NH2rGO-PAMAM nanoparticles in the prepared sensor films. The specificity, sensitivity, binding affinity, and selectivity of the SPR sensor were then evaluated. Results indicated that the variation of the sensing layer due to different spin speed, time incubation, and concentration provided a better interaction between the analyte and sensing layer. The linear dependence of the SPR sensor showed good linearity (R2 = 0.92) with the lowest detection of 0.08 pM DENV-2 E-proteins. By using the Langmuir model, the equilibrium association constant was obtained at very high value of 6.6844 TM-1 (R2 = 0.99). High selectivity of the SPR sensor towards DENV-2 E-proteins was achieved in the presence of other competitors.

Matched MeSH terms: Spectroscopy, Fourier Transform Infrared/methods

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