• 제목/요약/키워드: Ionization development

검색결과 187건 처리시간 0.027초

Development of Analytical Technology Using the HS-SPME-GC/FID for Monitoring Aromatic Solvents in Urine

  • Lee, Mi-Young;Chung, Yun Kyung;Shin, Kyong-Sok
    • Mass Spectrometry Letters
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    • 제4권1호
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    • pp.18-20
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    • 2013
  • Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

Identification of Protein Candidates in Porcine Oocytes during In Vitro Maturation

  • Lee, Jae-Dal;Cui, Xiang-Shun;Im, Gi-Sun;Seong, Hwan-Hoo;Kim, Nam-Hyung
    • Reproductive and Developmental Biology
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    • 제32권2호
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    • pp.71-79
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    • 2008
  • Surface-enhanced laser desorption and ionization time-of-flight mass spectrometry (SELDI-TOF MS) is one of the recently developed proteomic technologies which is based on capturing proteins and peptides by chemically modified surfaces and highly sensitive for the analysis of complex biological samples. In the present study, to gain insights into oocyte maturation and early embryo development, SELDI-TOF-MS was used to find the protein candidates that are specifically or prominently expressed in porcine oocytes at the in vitro matured metaphase II (MIIl) and germinal vesicle (GV) stages. By selected CM10 chip, 16 candidates were found to be up-regulated in GV stage oocytes compared with in MII stage oocytes, their molecular weights were 8,180 (2 candidates), 10,226 (5 candidates), 15,767 (5 candidates) and 16,770 (4 candidates) Da respectively. And the expression of 29 candidates were higher in MII than in GV stage oocytes, their molecular weight were 10,832 (3 candidates), 17,743 (8 candidates), 20,122 (3 candidates), 22,131 (3 candidates), 24,857 (7 candidates) and 33,507 (5 candidates) Da, respectively. The expression of selected 13 candidates (0.2 and 1.0 % error tolerances) were analyzed using real time RT-PCR. The proteins that differentially regulated during oocyte in vitro maturation in the pigs may be potential biomarkers of oocyte maturation and quality.

에틸 이소시아네이트와 프로필 이소시아네이트의 GC/FID 분석 (The Determination of Ethyl Isocyanate and Propyl Isocyanate by GC/FID)

  • 이은정;유철;최홍순;박준호;윤주송;조영봉
    • Environmental Analysis Health and Toxicology
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    • 제15권1_2호
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    • pp.53-59
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    • 2000
  • The purpose of this study is the development of the simple and precise determination method of ethyl isocyanate (EIC) and propyl isocyanate (PIC) through derivatization using secondary aliphatic amines by gas chromatography with flame ionization detector. The urea derivatives are quantitatively and simultaneously derived from EIC and PIC with secondary aliphatic amines such as dipropylamine, dibutylamine. and dipentylamine in methylene chloride, and confirmed by thin layer chromatography and gas chromatography with mass selective detector. For GC/FID, according to the increasing carbon atom of the amines, the retention time and peak area of the urea derivatives are increased. The instrumental detection limits for EIC and PIC were about 23.3∼34.8 $\mu\textrm{g}$ and 21.6∼28.9 $\mu\textrm{g}$, respectively.

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전기전도도법을 이용한 우레아 농도 센서 개발 (Development of an Urea Sensor using Electric Conductivity Method)

  • 최병철;김계연;양주영;김화남
    • 동력기계공학회지
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    • 제15권2호
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    • pp.55-60
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    • 2011
  • The popularity of diesel engines is derived primarily from their higher thermal efficiency resulting from higher compression ratio. NOx removal from the diesel emissions is very important to meet stringent emission regulations. NOx emission from diesel engines is removed by an urea-SCR or an LNT system. The urea-SCR system needs the urea-solution supply system with concentration and level sensor. This study was carried out to develop a sensor for the measurement of urea-solution concentration by an electric conductivity method. Considering experimental parameters were the material of electrode, two kinds of electric power(AC or DC), the distance between two electrodes, and the length of electrode. It was found that the AC electric power was more useful to measure the urea-solution concentration compared to DC, because it prevented an ionization of the urea-solution. The silver rod coated with Pt is the most useful electrode, tendency of which is similar to Pt rod, and the cost is more economic. We could also find out the optimum distance between two electrodes and the length of electrode was 10mm and 3mm, respectively.

Quantitative and Qualitative Analysis of Alkaloids in Coptis chinensis (Coptidis Rhizoma) by LC-DAD and LC-ESI/MS

  • Yu, Young-Beob;Bae, Chang-Hyu
    • 한국자원식물학회지
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    • 제30권6호
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    • pp.693-698
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    • 2017
  • The quality control of natural products is principal key to guarantee the Good Manufacturing Practices (GMP) and Good Clinical Practices (GCP) for the functional food, pharmaceuticals and cosmeceuticals in the industry. In this study, we examined the quantitative analysis of berberine as marker substance of Coptidis Rhizoma by high performance liquid chromatography-photodiode array detector (HPLC-DAD). The HPLC method was validated and met all the requirements for the quality control analysis recommended by FDA and ICH. The berberine was separated on a Xterra $C_{18}$ column ($5{\mu}m$, $4.6{\times}250mm$) using mobile phase consisting of distilled water and acetonitrile with $KH_2PO_4$ (3.4 g) and $Na_2SO_4$ (1.7 g). Calibration curve of berberine has been estimated (y = 42293.47x-41589 with the correlation coefficient 0.9999). The amount of berberine was calculated as 4.25%. And berberastine, palmatine, columbamine, jatrorrhizine, epiberberine, berberine and coptisine in the Coptidis Rhizoma were identified by high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-ESI-MS) method.

Pancastatin A and B Have Selective Cytotoxicity on Glucose-Deprived PANC-1 Human Pancreatic Cancer Cells

  • Park, Hae-Ryong
    • Journal of Microbiology and Biotechnology
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    • 제30권5호
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    • pp.733-738
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    • 2020
  • Glucose deprivation and hypoxia frequently occur in solid tumor cells, including pancreatic cancer cells. Glucose deprivation activates the unfolded protein response (UPR) and causes the up-regulation of glucose-regulated protein 78 (GRP78). Induction of GRP78 has been shown to protect cancer cells. Therefore, shutting down of GRP78 expression may be a novel strategy in anticancer drug development. Based on this understanding, a screening system established for anticancer agents that exhibit selective cytotoxicity on pancreatic cancer cells under glucose-deprived conditions. To test this hypothesis, the new compounds isolated, pancastatin A (PST-A) and B (PST-B), from Ponciri Fructus. PST-A and B were identified as glabretal triterpenoid moieties by electrospray ionization mass spectrometry and nuclear magnetic resonance spectroscopic methods. PST-A and B suppressed the accumulation of the UPR hallmark gene, GRP78, during glucose deprivation. Furthermore, PST-A and B showed selective cytotoxicity on PANC-1 pancreatic cancer cells under glucose deprivation. Interestingly, PST-A and B had no effect on these cells under normal growth conditions. Our results suggest that PST-A and B act as novel therapeutic agents to induce selective cell death in glucose-deprived pancreatic cancer cells.

Standardizing GC-FID Measurement of Nonmethane Hydrocarbons in Air for International Intercomparison Using Retention Index and Effective Carbon Number Concept

  • Liaw, Sheng-Ju;Tso, Tai-Ly
    • 분석과학
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    • 제8권4호
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    • pp.807-814
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    • 1995
  • Accurate measurements of ozone precursors are required to understand the process and extent of ozone formation in rural and urban areas. Nonmethane hydrocarbons (NMHCs) have been identified as important ozone precursors. Identification and quantification of NMHCs are difficult because of the large number present and the wide molecular weight range encountered in typical air samples. A major plan of the research team of the Climate and Air Quality Taiwan Station (CATs) was the measurement of atmospheric nonmethane hydrocarbons. An analytical method has been development for the analysis of the individual nonmethane hydrocarbons in ambient air at ppb (v) and subppb(v) levels. The whole ambient air samples were collected in canisters and analyzed by GC-FID with $Al_2O_3$/KCl PLOT column. Our targeted for quantitative analysis 43 compounds that may be substantial contributors to ozone formation. The retention indices and molar response factors of some commercially available $C_2{\sim}C_{10}$ hydrocarbons were determined and used to identify and quantify air samples. A quality assurance program was instituted to ensure that good measurements were made by participating in the International Nonmethane Hydrocarbon Intercomparison Experiments (NOMHICE).

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Rapid Determination of L-carnitine in Infant and Toddler Formulas by Liquid Chromatography Tandem Mass Spectrometry

  • Ahn, Jang-Hyuk;Kwak, Byung-Man;Park, Jung-Min;Kim, Na-Kyeoung;Kim, Jin-Man
    • 한국축산식품학회지
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    • 제34권6호
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    • pp.749-756
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    • 2014
  • A rapid and simple analytical method for L-carnitine was developed for infant and toddler formulas by liquid chromatography tandem mass spectrometry (LC-MS/MS). A 0.3 g of infant formula and toddler formula sample was mixed in a 50 mL conical tube with 9 mL water and 1 mL 0.1 M hydrochloric acid (HCl) to chemical extraction. Then, chloroform was used for removing a lipid fraction. After centrifuged, L-carnitine was separated and quantified using LC-MS/MS with electrospray ionization (ESI) mode. The precursor ion for L-carnitine was m/z 162, and product ions were m/z 103 (quantitative) and m/z 85 (qualitative), respectively. The results for spiked recovery test were in the range of 93.18-95.64% and the result for certified reference material (SRM 1849a) was within the range of the certificated values. This method could be implemented in many laboratories that require time and labor saving.

기체크로마토그래피를 이용한 식이보충제에서 메틸설포닐메탄의 검증된 분석법 개발 (Development of a Validated Determination of Methylsulfonylmethane in Dietary Supplement by Gas Chromatography)

  • 박상욱;이원재
    • KSBB Journal
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    • 제30권4호
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    • pp.141-147
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    • 2015
  • The convenient determination of methylsulfonylmethane (MSM) for a commercially available dietary supplement was developed using gas chromatography (GC)-flame ionization detector (FID). Chromatography was performed on a capillary column ($0.32mm\;I.D{\times}30m$, $0.25{\mu}m$) coated with dimethylpolysiloxane using diethylene glycol methyl ether as an internal standard. The performance characteristics of GC were evaluated in terms of selectivity, linearity, precision, accuracy, recovery, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination: 0.9979) within the concentration range of $10.0{\sim}800.0{\mu}g/mL$ for MSM. The recoveries for three fortified concentrations were 96.7~97.1%, 96.6~97.3% and 96.8~97.2%, respectively. The LOD and LOQ of the method were $0.29{\mu}g/mL$ and $0.97{\mu}g/mL$, respectively. All obtained results were acceptable according to the guidelines of the Association of Official Analytical Chemists for dietary supplements. Thus, the validated analytical method using the GC-FID system is suitable for the determination of MSM in dietary supplement formulations for quality control.

Design and development of enhanced criticality alarm system for nuclear applications

  • Srinivas Reddy, Padi;Kumar, R. Amudhu Ramesh;Mathews, M. Geo;Amarendra, G.
    • Nuclear Engineering and Technology
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    • 제50권5호
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    • pp.690-697
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    • 2018
  • Criticality alarm systems (CASs) are mandatory in nuclear plants for prompt alarm in the event of any criticality incident. False criticality alarms are not desirable as they create a panic environment for radiation workers. The present article describes the design enhancement of the CAS at each stage and provides maximum availability, preventing false criticality alarms. The failure mode and effect analysis are carried out on each element of a CAS. Based on the analysis, additional hardware circuits are developed for early fault detection. Two different methods are developed, one method for channel loop functionality test and another method for dose alarm test using electronic transient pulse. The design enhancement made for the external systems that are integrated with a CAS includes the power supply, criticality evacuation hooter circuit, radiation data acquisition system along with selection of different soft alarm set points, and centralized electronic test facility. The CAS incorporating all improvements are assembled, installed, tested, and validated along with rigorous surveillance procedures in a nuclear plant for a period of 18,000 h.