• Title/Summary/Keyword: High-resolution mass spectrometry

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SIMS Study on the Diffusion of Al in Si and Si QD Layer by Heat Treatment

  • Jang, Jong Shik;Kang, Hee Jae;Kim, An Soon;Baek, Hyun Jeong;Kim, Tae Woon;Hong, Songwoung;Kim, Kyung Joong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.188.1-188.1
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    • 2014
  • Aluminum is widely used as a material for electrode on silicon based devices. Especially, aluminum films are used as backside and front-side electrodes in silicon quantum dot (QD) solar cells. In this point, the diffusion of aluminum is very important for the enhancement of power conversion efficiency by improvement of contact property. Aluminum was deposited on a Si (100) wafer and a Si QD layer by ion beam sputter system with a DC ion gun. The Si QD layer was fabricated by $1100^{\circ}C$ annealing of the $SiO_2/SiO_1$ multilayer film grown by ion beam sputtering deposition. Cs ion beam with a low energy and a grazing incidence angle was used in SIMS depth profiling analysis to obtain high depth resolution. Diffusion behavior of aluminum in the Al/Si and Al/Si QD interfaces was investigated by secondary ion mass spectrometry (SIMS) as a function of heat treatment temperature. It was found that aluminum is diffused into Si substrate at $450^{\circ}C$. In this presentation, the effect of heat treatment temperature and Si nitride diffusion barrier on the diffusion of Al will be discussed.

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Diffusion Behaviors and Electrical Properties in the In-Ga-Zn-O Thin Film Deposited by Radio-frequency Reactive Magnetron Sputtering

  • Lee, Seok Ryeol;Choi, Jae Ha;Lee, Ho Seong
    • Journal of the Korean institute of surface engineering
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    • v.48 no.6
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    • pp.322-328
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    • 2015
  • We investigated the diffusion behaviors, electrical properties, microstructures, and composition of In-Ga-Zn-O (IGZO) oxide thin films deposited by radio frequency reactive magnetron sputtering with increasing annealing temperatures. The samples were deposited at room temperature and then annealed at 300, 400, 500, 600 and $700^{\circ}C$ in air ambient for 2 h. According to the results of time-of-flight secondary ion mass spectrometry and X-ray photoelectron spectroscopy, no diffusion of In, Ga, and Zn components were observed at 300, 400, 500, $600^{\circ}C$, but there was a diffusion at $700^{\circ}C$. However, for the sample annealed at $700^{\circ}C$, considerable diffusion occurred. Especially, the concentration of In and Ga components were similar at the IGZO thin film but were decreased near the interface between the IGZO and glass substrate, while the concentration of Zn was decreased at the IGZO thin film and some Zn were partially diffused into the glass substrate. The high-resolution transmission electron microscopy results showed that a phase change at the interface between IGZO film and glass substrate began to occur at $500^{\circ}C$ and an unidentified crystalline phase was observed at the interface between IGZO film and glass substrate due to a rapid change in composition of In, Ga and Zn at $700^{\circ}C$. The best values of electron mobility of $15.5cm^2/V{\cdot}s$ and resistivity of $0.21{\Omega}cm$ were obtained from the sample annealed at $600^{\circ}C$.

A comparative study on chemical composition of total saponins extracted from fermented and white ginseng under the effect of macrophage phagocytotic function

  • Xiao, Dan;Xiu, Yang;Yue, Hao;Sun, Xiuli;Zhao, Huanxi;Liu, Shuying
    • Journal of Ginseng Research
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    • v.41 no.3
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    • pp.379-385
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    • 2017
  • In this study, white ginseng was used as the raw material, which was fermented with Paecilomyces hepiali through solid culture medium, to produce ginsenosides with modified chemical composition. The characteristic chemical markers of the products thus produced were investigated using rapid resolution liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (RRLC-QTOF-MS). Chemical profiling data were obtained, which were then subjected to multivariate statistical analysis for the systematic comparison of active ingredients in white ginseng and fermented ginseng to understand the beneficial properties of ginsenoside metabolites. In addition, the effects of these components on biological activity were investigated to understand the improvements in the phagocytic function of macrophages in zebrafish. According to the established RRLC-QTOF-MS chemical profiling, the contents in ginsenosides of high molecular weight, especially malonylated protopanaxadiol ginsenosides, were slightly reduced due to the fermentation, which were hydrolyzed into rare and minor ginsenosides. Moreover, the facilitation of macrophage phagocytic function in zebrafish following treatment with different ginseng extracts confirmed that the fermented ginseng is superior to white ginseng. Our results prove that there is a profound change in chemical constituents of ginsenosides during the fermentation process, which has a significant effect on the biological activity of these compounds.

Synthesis of Curcumin Glycosides with Enhanced Anticancer Properties Using One-Pot Multienzyme Glycosylation Technique

  • Gurung, Rit Bahadur;Gong, So Youn;Dhakal, Dipesh;Le, Tuoi Thi;Jung, Na Rae;Jung, Hye Jin;Oh, Tae Jin;Sohng, Jae Kyung
    • Journal of Microbiology and Biotechnology
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    • v.27 no.9
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    • pp.1639-1648
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    • 2017
  • Curcumin is a natural polyphenolic compound, widely acclaimed for its antioxidant, anti-inflammatory, antibacterial, and anticancerous properties. However, its use has been limited due to its low-aqueous solubility and poor bioavailability, rapid clearance, and low cellular uptake. In order to assess the effect of glycosylation on the pharmacological properties of curcumin, one-pot multienzyme (OPME) chemoenzymatic glycosylation reactions with UDP-${\alpha}-{\text\tiny{D}}$-glucose or UDP-${\alpha}-{\text\tiny{D}}$-2-deoxyglucose as donor substrate were employed. The result indicated significant conversion of curcumin to its glycosylated derivatives: curcumin 4'-O-${\beta}$-glucoside, curcumin 4',4"-di-O-${\beta}$-glucoside, curcumin 4'-O-${\beta}$-2-deoxyglucoside, and curcumin 4',4"-di-O-${\beta}$-2-deoxyglucoside. The products were characterized by ultra-fast performance liquid chromatography, high-resolution quadruple-time-of-flight electrospray ionization-mass spectrometry, and NMR analyses. All the products showed improved water solubility and comparable antibacterial activities. Additionally, the curcumin 4'-O-${\beta}$-glucoside and curcumin 4'-O-${\beta}$-2-deoxyglucoside showed enhanced anticancer activities compared with the parent aglycone and diglycoside derivatives. This result indicates that glycosylation can be an effective approach for enhancing the pharmaceutical properties of different natural products, such as curcumin.

In Vitro Wheat Immature Spike Culture Screening Identified Fusarium Head Blight Resistance in Wheat Spike Cultured Derived Variants and in the Progeny of Their Crosses with an Elite Cultivar

  • Huang, Chen;Gangola, Manu P.;Kutcher, H. Randy;Hucl, Pierre;Ganeshan, Seedhabadee;Chibbar, Ravindra N.
    • The Plant Pathology Journal
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    • v.36 no.6
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    • pp.558-569
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    • 2020
  • Fusarium head blight (FHB) is a devastating fungal disease of wheat (Triticum aestivum L.). The lack of genetic resources with stable FHB resistance combined with a reliable and rapid screening method to evaluate FHB resistance is a major limitation to the development of FHB resistant wheat germplasm. The present study utilized an immature wheat spike culture method to screen wheat spike culture derived variants (SCDV) for FHB resistance. Mycotoxin concentrations determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS) correlated significantly (P < 0.01) with FHB severity and disease progression during in vitro spike culture. Selected SCDV lines assessed for FHB resistance in a Fusarium field disease nursery in Carman, Manitoba, Canada in 2016 showed significant (P < 0.01) correlation of disease severity to the in vitro spike culture screening method. Selected resistant SCDV lines were also crossed with an elite cv. CDC Hughes and the progeny of F2 and BC1F2 were screened by high resolution melt curve (HRM) analyses for the wheat UDP-glucosyl transferase gene (TaUGT-3B) single nucleotide polymorphism to identify resistant (T-allele) and susceptible (G-allele) markers. The progeny from the crosses were also screened for FHB severity using the immature spike culture method and identified resistant progeny grouped according to the HRM genotyping data. The results demonstrate a reliable approach using the immature spike culture to screen for FHB resistance in progeny of crosses in early stage of breeding programs.

Qualitative Analysis for Metabolites of Pharmaceuticals Formed in Daphnia magna and Gammarus pulex Using Liquid Chromatogram-High Resolution Mass Spectrometry (LC-HRMS) (LC-HRMS를 이용한 Daphnia magna 및 Gammarus pulex 생체내 의약품 대사체 정성분석)

  • Jeon, Junho
    • Journal of Environmental Analysis, Health and Toxicology
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    • v.21 no.4
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    • pp.243-251
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    • 2018
  • Pharmaceuticals in wastewater effluents have been recognized as emerging pollutants threatening freshwater organisms. To extend understanding for bioaccumulation and toxicity in those organisms, information on biotransformation products (or metabolites) and their metabolic pathway are crucial. The aim of the present study is to identify and elucidate metabolites of pharmaceuticals formed in exposed organisms using suspect and nontarget screening approach using LC-HRMS. As the target pharmaceuticals, carbamazepine, ketoprofen, metoprolol, propranolol, and verapamil were selected whereas Daphnia magna and Gammarus pulex were used as test organisms. After 24h exposure, metabolites formed in the organisms were identified using LC-HRMS. The structures of metabolites were elucidated via analysis of MS/MS fragment pattern and the comparison with fragment database. As the results, a total of 10 metabolites were identified for 5 parent compounds (C253/C356 for carbamazepine, K211 for ketoprofen, M256 for metoprolol, P218/P276/P306 for propranolol, V196/V291/V441 for verapamil). Among them, the presence of C253 and V291 was confirmed using standard materials. Most of the identified metabolites were formed through oxidative reactions such as hydroxylation, N-demethylation, and dealkylation. Cysteine conjugation (phase II reaction) metabolite (C356) for carbamazepine was found in daphnia. The metabolic pathway of verapamil showed similar metabolic pathways and metabolic pathways for both species. Although the toxicological information on the identified metabolites could not be confirmed, the molecular structure information of the proposed metabolites can be used for future evaluation and prediction of toxicity.

A review on status of organic micropollutants from sewage effluent and their management strategies (하수 유래 미량오염물질 현황과 관리 방안 고찰)

  • Choi, Sangki;Lee, Woongbae;Kim, Young-Mo;Hong, Seok-Won;Son, Heejong;Lee, Yunho
    • Journal of Korean Society of Water and Wastewater
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    • v.35 no.3
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    • pp.205-225
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    • 2021
  • Due to the large-scale production and use of synthetic chemicals in industralized countries, various chemicals are found in the aquatic environment, which are often termed as micropollutants. Effluents of municipal wastewater treatment plants (WWTPs) have been identified as one of the major sources of these micropollutants. In this article, the current status of occurrence and removal of micropollutants in WWTPs and their management policies and options in domestic and foregin countries were critically reviewed. A large number of pharmaceuticals, personal care products, and industrial chemicals are found in WWTPs' influent, and are only partially removed by current biological wastewater treatment processes. As a result, some micropollutants are present in WWTPs' effluents, which can negatively affect receiving water quality or drinking water source. To better understand and assess the potential risk of micropollutants, a systematic monitoring framework including advanced analytical tools such as high resolution mass spectrometry and bioanalytical methods is needed. Some Western European countries are taking proactive approach to controlling the micropollutants by upgrading WWTP with enahnced effluent treatment processes. While this enahnced WWTP effluent treatment appears to be a viable option for controlling micropollutant, its implementation requires careful consideration of the technical, economical, political, and cultural issues of all stakeholders.

Alpha-Glucosidase Inhibitory Activity of Saponins Isolated from Vernonia gratiosa Hance

  • Pham Van Cong;Hoang Le Tuan Anh;Le Ba Vinh;Yoo Kyong Han;Nguyen Quang Trung;Bui Quang Minh;Ngo Viet Duc;Tran Minh Ngoc;Nguyen Thi Thu Hien;Hoang Duc Manh;Le Thi Lien;Ki Yong Lee
    • Journal of Microbiology and Biotechnology
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    • v.33 no.6
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    • pp.797-805
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    • 2023
  • Species belonging to the Vernonia (Asteraceae), the largest genus in the tribe Vernonieae (consisting of about 1,000 species), are widely used in food and medicine. These plants are rich sources of bioactive sesquiterpene lactones and steroid saponins, likely including many as yet undiscovered chemical components. A phytochemical investigation resulted in the separation of three new stigmastane-type steroidal saponins (1 - 3), designated as vernogratiosides A-C, from whole plants of V. gratiosa. Their structures were elucidated based on infrared spectroscopy (IR), one-dimensional (1D) and two-dimensional nuclear magnetic resonance (2D NMR), high-resolution electrospray ionization mass spectrometry (HR-ESI-MS), and electronic circular dichroism analyses (ECD), as well as chemical reactivity. Molecular docking analysis of representative saponins with α-glucosidase inhibitory activity was performed. Additionally, the intended substances were tested for their ability to inhibit α-glucosidase activity in a laboratory setting. The results suggested that stigmastane-type steroidal saponins from V. gratiosa are promising candidate antidiabetic agents.

Identification and Quantification of Phenolic Acid Derivatives from Three Korean White and Brown Rice Samples Based on High-Resolution Mass Spectrometry (쌀(백미, 현미) 시료로부터 고해상도 질량 분석 기반의 페놀산 유도체 동정 및 정량 평가)

  • Hyemin Na;Ryeong Ha Kwon;Ju Hyung Kim;So Ah Kim;Soo-Muk Cho;Heon-Woong Kim
    • The Korean Journal of Food And Nutrition
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    • v.36 no.6
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    • pp.506-514
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    • 2023
  • Reported positive ion fragmentation of phenolic acid derivatives in rice (Oryza sativa L.) were summarized based on the literature. A total of eight phenolic acids (4 derivatives of ferulic acid, 3 derivatives of sinapic acid and p-coumaric acid) were isolated and identified from rice (raw and steamed) using UPLC-DAD-QToF/MS. Results revealed that 6-O-feruloylsurose was the major component with 3'-O-sinapoylsucorse being tentatively identified in Oryza sativa L. for the first time as a new hydroxycinnamoyl derivative in rice grains. In our study, raw brown rice had the highest phenolic acid contents with Samkwang showing higher phenolic acid content than Saeilmi and Sindongjin (12.41 vs. 7.89 and 3.10 mg/100 g dry weight, respectively). Of all varieties, brown rice had higher phenolic acid contents than white rice. These contents decreased considerably when rice was steamed whereas, p-coumaric acid and ferulic acid contents were increased. Additionally, contents of rice (raw and steamed) can be used as a fundamental report for new rice varieties.

Structural evaluation of degradation products of Loteprednol using LC-MS/MS: Development of an HPLC method for analyzing process-related impurities of Loteprednol

  • Rajesh Varma Bhupatiraju;Bikshal Babu Kasimala;Lavanya Nagamalla;Fathima Sayed
    • Analytical Science and Technology
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    • v.37 no.2
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    • pp.98-113
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    • 2024
  • The current investigation entails the characterization of five degradation products (DPs) formed under different stress conditions of loteprednol using liquid chromatography-tandem mass spectrometry (LC-MS/MS). In addition, this study developed a stable high-performance liquid chromatography (HPLC) method for evaluating loteprednol along with impurities. The method conditions were meticulously fine-tuned which involved the exploration of the appropriate solvent, pH, flow of the mobile phase, columns, and wavelength. The method conditions were carefully chosen to successfully resolve the impurities of loteprednol and were employed in subsequent validation procedures. The stability profile of loteprednol was exposed to stress degradation experiments conducted under five conditions, and DPs were structurally characterized by employing LC-MS/MS. The chromatographic resolution of loteprednol and its impurities along with DPs was effectively achieved using a Phenomenex Luna 250 mm C18 column using 0.1 % phosphoric acid, methanol, and acetonitrile in 45:25:30 (v/v) pumped isocratically at 0.8 mL/min with 243 nm wavelength. The method produces an accurate fit calibration curve in 50-300 ㎍/mL for loteprednol and LOQ (0.05 ㎍/mL) - 0.30 ㎍/mL for its impurities with acceptable precision, accuracy, and recovery. The stress-induced degradation study revealed the degradation of loteprednol under basic, acidic, and photolytic conditions, resulting in the formation of seven distinct DPs. The efficacy of this method was validated through LC-MS/MS, which allowed for the verification of the chemical structures of the newly generated DPs of loteprednol. This method was appropriate for assessing the impurities of loteprednol and can also be appropriate for structural and quantitative assessment of its degradation products.