• Title/Summary/Keyword: Degradation products

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Degradation Efficiency and Characterization of Lincomycin by Electron Beam Irradiation

  • Ham, Hyun-Sun;Cho, Hyun-Woo;Myung, Seung-Woon
    • Mass Spectrometry Letters
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    • v.5 no.3
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    • pp.89-93
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    • 2014
  • Lincomycin is one of the major species among the Pharmaceuticals and Personal Care Products (PPCPs) detected from the four major rivers in Korea. The structure characterization was performed of six degradation products of lincomycin formed under the irradiation of electron beam, and the degradation efficiency as a function of the various irradiation dose and sample concentration was investigated. Electron beam (10 MeV, 0.5 mA and 5 kW) experiments for the structural characterization of degradation products that are fortified with lincomycin, were performed at the dose of 10 kGy. The separation of degradation products and lincomycin was carried out using a C18 column ($2.1{\times}100$ mm, $3.5{\mu}m$), using gradient elution with 20 mM ammonium acetate and acetonitrile. The structures of six degradation products of lincomycin were proposed by interpretation of mass spectra and chromatograms by LC-MS/MS. The mass fragmentation pathways of mass spectra in tandem mass spectrometry were also proposed. Experiments were performed of the degradation efficiency as a function of the irradiation dose intensity and the initial concentration of lincomycin in an aqueous environment. In addition, increased degradation efficiency was observed with a higher dose of electron beam and lower concentration.

A Scientific Analytical on the Ancient Shipwrecks Degradation Products Excavated from Underwater: Focused on Sulfur and Iron Degradation Products

  • Ji-Seon SONG;Yong-Hee YOON;Chang-Hyun PARK
    • Journal of the Korean Wood Science and Technology
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    • v.52 no.3
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    • pp.243-261
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    • 2024
  • In this study, samples were collected from various ancient wooden shipwrecks, including the Shinan shipwreck and Jindo shipwreck that used iron nails, the Yeongheungdo shipwreck carrying iron artifacts, as well as the Sibidongpado shipwreck and Wando shipwreck where degradation products were not observed, all of which were salvaged by the National Research Institute of Maritime Heritage. The aim was to analyze the characteristics of degradation products generated by iron (Fe) within the salvaged wooden shipwreck materials and establish fundamental data on degradation products in waterlogged archaeological wood. The analysis revealed that sulfur (S) is generally accumulated in wood obtained from marine environments. It was observed that the content of inorganic substances such as iron and sulfur was significantly higher in the Shinan shipwreck, Jindo shipwreck, and Yeongheungdo shipwreck compared to Sibidongpado shipwreck and Wando shipwreck, which used wooden nails. This indicates that the presence of iron affects the accumulation of degradation products and suggests that iron is a factor in the corrosion of wood. Furthermore, crystallin compounds were observed within the cell walls, and higher concentrations of iron and sulfur were found in the resin ducts, rays, and radial tissues. This suggests that during desalination and consolidation treatments, warm water or polyethylene glycol (PEG) may move degradation factors into resincanals, rays, radial tissues, etc.

Characterization of Thermal Products of Alpha-Tocopherol

  • Chung, Hee-Young
    • Preventive Nutrition and Food Science
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    • v.9 no.4
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    • pp.295-299
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    • 2004
  • Alpha-tocopherol was thermally oxidized and degraded at high temperatures and the resulting products were chromatographically separated and identified by LC-MS. Alpha-tocopherol dissolved in glycerol was heated at 200^{\circ}C for 30 min. The thermal products were separated by hexane extraction and analyzed by HPLC using a reversed phase $\mu$-Bondapak $C_{18}-column$ with two kinds of elution solvents: a mixture of acetonitrile and methanol (3:2), and of acetonitrile, methanol, 2-propanol, chloroform and methylene chloride (3:2:5:0.5:0.5) in a gradient mode. The isolated thermal. products of alpha-tocopherol were more viscous than alpha-tocopherol, and dark brown in color. Major thermal degradation products of alpha-tocopherol were identified by LC-MS, and the structures of thermal products were proposed. Alpha-tocopherol and its thermal degradation products were degraded into fragments, mainly at the non-aromatic parts. The degradation products of alpha-tocopherol. were combined with oxidized product (tocopherylquinone) to make thermal. products through dimerization.

GC-MS Analysis of Amur Cork Tree Extract and Its Degradation Products

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.34 no.6
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    • pp.1042-1052
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    • 2010
  • The Degradation of amur cork tree extract is investigated by GC-MS after treating the dye with three thermal degradation systems of, room temperature (RT), $4^{\circ}C$ refrigeration (LT), $100^{\circ}C$ oven (OV), and $H_2O_2$/UV/$O_2$ (PER) degradation system for 0-24 days. It was found that PER degradation system represented the highest intensity of degradation treatment followed by OV treatment among the four degradation parameters. The possible fingerprint products of amur cork tree dye, that yielded 68% (or higher) reliability in the NIST spectral match, were isobenzofuran-1,3-dione,4,5-dimethoxy- (8.37 min, PER only), 1,3-dioxolo[4,5-g]isoquinolin-5(6H)-one,7,8-dihydro (9.41 min, PER only), canthine-6-one (10.24 min, RT, LT, OV only), and dihydroberberine (15.05 min, RT, LT, OV, PER) in the order of higher to lower possibility of detection. Unknown products 7 (13.43 min) and 8 (16.35 min) are two other possible fingerprint products of amur cork tree dye that require future identification.

DEGRADATION OF NUCLEIC ACIDS BY CELL-FREE EXTRACT OF MIXED RUMEN PROTOZOA OF BUFFALO RUMEN

  • Sinha, P.R.;Dutta, S.M..
    • Asian-Australasian Journal of Animal Sciences
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    • v.1 no.4
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    • pp.219-222
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    • 1988
  • Degradation of deoxyribonucleic acid(DNA) and ribonucleic acid(RNA) by cell-free extract of mixed rumen protozoa of buffalo rumen was investigated. DNA was observed to be degraded rapidly during an initial incubation period of 2 hr with simultaneous appearance of degradation products. RNA on the other hand recorded a rapid degradation during an initial incubation period of 1 hr. RNA degradation products appeared upto an incubation period of 2 hr. DNA was observed to degrade into oligo- and mononucleotides. pyrimidine nucleosides, purine nucleoside adenosine and bases xanthine, hypoxanthine and thymine. Degradation products of RNA comprised of pyrimidine nucleosides, purine nucleoside, adenosine and bases xanthine, hypoxanthine and uracil besides oligo- and mononucleotides.

Establishing and validating an HPLC protocol for pralsetinib impurities analysis, coupled with HPLC-MS/MS identification of stress degradation products

  • Rajesh Varma Bhupatiraju;Pavani Peddi;Venkata Swamy Tangeti;Battula Sreenivasa Rao
    • Analytical Science and Technology
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    • v.37 no.5
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    • pp.280-294
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    • 2024
  • This study introduces a novel analytical method for the assessment of pralsetinib impurities and degradation products (DPs), addressing critical gaps in existing methodologies. This research aims to develop a robust HPLC method for impurity analysis, characterize degradation products using LC-MS, and evaluate the environmental impact of the method. The study began by optimizing HPLC conditions with various columns and buffers, ultimately achieving successful separation using an XBridge® RP-C18 column with ethanol as solvent A and 50 mM formic acid at pH 2.9. This setup provided excellent peak resolution and symmetry, essential for reliable stability studies. The developed HPLC method was then adapted for HPLC-MS/MS, enhancing sensitivity and detection efficiency of DPs. Stress degradation studies of pralsetinib under different conditions (acidic, basic, oxidative, thermal, and photolytic) revealed significant degradation under acidic (29.3 %) and basic (21.5 %) conditions, with several DPs identified. Oxidative stress resulted in 19.8 % degradation, while thermal and photolytic conditions caused minimal degradation. HPLC-MS/MS analysis identified structures of five degradation products, providing detailed insights into pralsetinib's stability and degradation pathways. Method validation followed ICH guidelines Q2(R1), confirming method's specificity, selectivity, sensitivity, linearity, accuracy, precision, and robustness. The method exhibited strong linearity with a coefficient of determination (r2) greater than 0.999 for pralsetinib and its impurities. This method advances impurity detection and DPs characterization, ensuring the quality and safety of pralsetinib. Additionally, method's environmental impact was assessed, aligning with sustainable analytical practices. These findings provide essential data on pralsetinib's stability, guiding storage conditions and ensuring its efficacy and safety in pharmaceutical applications.

Kinetics of Thermal Degradation of Polypropylene/Nanoclay/Wood Flour Nanocomposites

  • Mohan, D. Jagan;Lee, Sun-Young;Kang, In-Aeh;Doh, Geum-Hyun;Park, Byung-Dae;Wu, Qinglin
    • Journal of the Korean Applied Science and Technology
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    • v.24 no.3
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    • pp.278-286
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    • 2007
  • As a part of enhancing the performance of wood-plastic composites (WPC), polypropylene (PP)/ nanoclay (NC)/ wood flour (WF) nanocomposites were prepared using melt blending and injection molding process to evaluate their thermal stability. Thermogravimetric analysis (TGA) was employed to investigate thermal degradation kinetics of the nanocomposites both dynamic and isothermal conditions. Dynamic scans of the TGA showed an increased thermal stability of the nanocomposites at moderate wood flour concentrations (up to 20 phr, percentage based on hundred percent resin) while it decreased with the addition of 30 phr wood flour. The activation energy $(E_a)$ of thermal degradation of nanocomposites increased when nanoclay was added and the concentration of wood flour increased. Different equations were used to evaluate isothermal degradation kinetics using the rate of thermal degradation of the composites, expressed as weight loss (%) from their isothermal TGA curves. Degradation occurred at faster rate in the initial stages of about 60 min., and then proceeded in a gradual manner. However, nanocomposites with wood flour of 30 phr heated at $300^{\circ}C$ showed a drastic difference in their degradation behavior, and reached almost a complete decomposition after 40 min. of the isothermal heating. The degree of decomposition was greater at higher temperatures, and the residual weight of isothermal degradation of nanocomposites greatly varied from about 10 to 90%, depending on isothermal temperatures. The isothermal degradation of nanocomposites also increased their thermal stability with the addition of 1 phr nanoclay and of wood flour up to 20 phr. But, the degradation of PP100/NC1/MAPP3/WF30 nanocomposites with 30 phr wood flour occurs at a faster rate compared to those of the others, indicating a decrease in their thermal stability.

Thermal Degradation of Aqueous MEA Solution for CO2 Absorption by Nuclear Magnetics Resonance (핵자기공명분석법을 이용한 수용성 아민 CO2 흡수제인 MEA의 열적변성 분석)

  • CHOI, JEONGHO;YOON, YEOIL;PARK, SUNGYOUL;BAEK, ILHYUN;KIM, YOUNGEUN;NAM, SUNGCHAN
    • Journal of Hydrogen and New Energy
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    • v.27 no.5
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    • pp.562-570
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    • 2016
  • At the carbon dioxide capture process using the aqueous amine solution, degradation of absorbents is main factor to reducing the process performance. Also, degradation mechanism of absorbent is important for understanding the environmental risk, route of degradation products, health risk etc. In this study, the degradation products of MEA were studied to clarify mechanism in thermal degradation process. The degradation products were analyzed using a $^1H$ NMR (nuclear magnetic resonance) and $^{13}C$ NMR. The analysis methods used in this study provide guidelines that could be used to develop a degradation inhibitor of absorbent and a corrosion inhibitor.

Identification of Degradation Products in the Phosphodiesterase (PDE-4) Inhibitor Roflumilast Using High Resolution Mass Spectrometry and Density Functional Theory Calculations

  • Paul, Saroj Kumar;Dash, Upendra N.
    • Mass Spectrometry Letters
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    • v.6 no.2
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    • pp.38-42
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    • 2015
  • Roflumilast analogs are a group of drugs which act as selective photodiesterase (PDE-4) inhibitor for the treatment severe chronic pulmonary disease associated with chronic brochnonities. Structural identification of degradation products using high resolution mass spectrometry and theoretical investigation by density functional theory have been successfully carried out on roflumilast to identify four degradation products namely, 3,5-dichloropyridin-4-amine, N-(3,5-dichloropyridin-4-yl)-4-(difluoromethoxy)-3-hydroxy benzamide, N-(3,5-dichloropyridin-4-yl)-3-(cyclopropylmethoxy)-4-(difluoromethoxy) benzamide and 3-(cyclopropylmethoxy)-N-(3,5-dichloro-1-oxidopyridin-4-yl)-4-(difluoro methoxy) benzamide, generated in alkali, acidic and oxidative conditions.

Characterization of Thermal Degradation of Polytrimethylene Terephthalate by MALDI-TOF Mass Spectrometry

  • Jang, Sung-Woo;Yang, Eun-Kyung;Jin, Sung-Il;Cho, Young-Dal;Choe, Eun-Kyung;Park, Chan-Ryang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.3
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    • pp.833-838
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    • 2012
  • The thermal degradation products of polytrimethylene terephthalate (PTT) obtained by heating the sample in the temperature range of $250-360^{\circ}C$ under non-oxidative conditions was characterized using MALDI-TOF (matrix assisted laser desorption/ionization) mass spectrometry. The structures of the degradation products were determined and the relative compositions were estimated. The MALDI-TOF mass spectra of the thermally degraded PTT sample showed three main series of oligomer products with different end groups, which were carboxyl/carboxyl, carboxyl/allyl, and allyl/allyl. In contrast to the thermal degradation of polyethylene terephthalate (PET), the oligomers containing terephthalic anhydrides were not detected, whereas the formation of oligomers containing the unsaturated allyl ester group was confirmed by mass assignment. From these results, it was concluded that the thermal degradation of PTT proceeds exclusively through the ${\beta}$-CH hydrogen transfer mechanism, which is in accordance with the proposed reaction mechanism for the thermal degradation of polybutylene terephthalate (PBT).