• Title/Summary/Keyword: Dilution Mode

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Analysis of sorbic acid in tea-drink using isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS) (동위원소희석 액체 크로마토그래피-질량분석법을 이용한 차음료 중의 소르빈산의 분석)

  • Ahn, Seong-Hee;Lee, In-Sun;Kim, Byung-Joo
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.25-32
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    • 2012
  • Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

Accurate determination of chloramphenicol in meat by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS) (동위원소희석 액체크로마토그래피-질량분석법을 이용한 육류 중 클로람페니콜의 정밀한 정량 분석에 관한 연구)

  • Song, Hye-Min;Kim, Byung-Joo;Jeong, Hyuk;Ahn, Seong-Hee
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.524-530
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    • 2010
  • Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

Effect of Outdoor Temperature on the Refrigerant Behavior in the Compressor of a Heat Pump Operating at Heating Mode (열펌프의 난방운전시 외기온이 압측기의 냉매거동에 미치는 영향)

  • 이재효;김병균;이건우
    • Korean Journal of Air-Conditioning and Refrigeration Engineering
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    • v.16 no.5
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    • pp.452-458
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    • 2004
  • The major cause of compressor failure is the decrease of oil viscosity due to floodback. In most previous researches on the compressor reliability, the relationship between oil circulation rate and performance or oil viscosity has been studied. Another research topic is flow visualization by using a sight glass on the bottom of a compressor sump area and accumulator. Both oil film thickness and oil level through the sight glass should be assessed for compressor reliability if the oil content of the mixture is small and low viscosity raise poor lubrication of pump bearing. In this study, the compressor reliability was assessed by measuring the viscosity of the mixture and calculating oil film thickness. The analysis of the relationship between bottom shell super heat and oil film thickness at heating operation was peformed. It is concluded that bottom shell superheat does not perfectly stand for the mixture's behavior for a low ambient heating operation and oil film thickness can give more detailed and direct criteria for compressor reliability.

The Effect of Exhaust Gas Recirculation (EGR) on Combustion Stability, Engine Performance and Exhaust Emissions In a Gasoline Engine

  • Jinyoung Cha;Junhong Kwon;Youngjin Cho;Park, Simsoo
    • Journal of Mechanical Science and Technology
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    • v.15 no.10
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    • pp.1442-1450
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    • 2001
  • The EGR system has been widely used to reduce nitrogen oxides (NO$\_$x/) emission, to improve fuel economy and suppress knock by using the characteristics of charge dilution. However, as the EGR rate at a given engine operating condition increases, the combustion instability increases. The combustion instability increases cyclic variations resulting in the deterioration of engine performance and emissions. Therefore, the optimum EGR rate should be carefully determined in order to obtain the better engine performance and emissions. An experimental study has been performed to investigate the effects of EGR on combustion stability, engine performance,70x and the other exhaust emissions from 1.5 liter gasoline engine. Operating conditions are selected from the test result of the high speed and high acceleration region of SFTP mode which generates more NO$\_$x/ and needs higher engine speed compared to FTP-75 (Federal Test Procedure) mode. Engine power, fuel consumption and exhaust emissions are measured with various EGR rate. Combustion stability is analyzed by examining the variation of indicated mean effective pressure (COV$\_$imep/) and the timings of maximum pressure (P$\_$max/) location using pressure sensor. Engine performance is analyzed by investigating engine power and maximum cylinder pressure and brake specific fuel consumption (BSFC)

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Simultaneous Determination of Statins in Human Urine by Dilute-and-Shoot-Liquid Chromatography-Mass Spectrometry

  • Jang, Haejong;Mai, Xuan-Lan;Lee, Gunhee;Ahn, Jae Hyoung;Rhee, Jongsook;Truong, Quoc-Ky;Vinh, Dinh;Hong, Jongki;Kim, Kyeong Ho
    • Mass Spectrometry Letters
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    • v.9 no.4
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    • pp.95-99
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    • 2018
  • An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the "dilute and shoot" (DAS) approach enabled a fast and reliable analysis. The influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sensitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects.

Mutagenicity of Diesel-Exhaust Particulates

  • Yoo, Young S.
    • Journal of Korean Society for Atmospheric Environment
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    • v.10 no.E
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    • pp.325-331
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    • 1994
  • Organic extracts of diesel- exhaust particulates were analyzed for mutagenicity using Ames Salmonella typhimurium assay system. An experimental diesel microbus used was drived on the chassis dynamometer according to CVS-75 mode. The samples were taken from the mixed gases in a dilution tunnel. With a high-volume air sampler equipped with double filter holders, particulate matters were collected on a teflon-coated glass fiber filter placed behind a activated carbon filter. After ultrasonic extraction with benzene- ethanol and evaporation to dryness, the residue was dissolved in dimethylsulfoxide. Each sample was tested toward 2 strains, TA100 and TA98 by the pre-incubation method in the absence and presence of S-9mix. Average concentration of diesel- exhaust particulates was about 116.6mg/m$^3$, and 44.1~62.2 % to the total weight of particulates, consisted of organic matters. The mutagenicities of diesel- exhaust particulate organic matters were 4,512 and 2,205 revertants/m$^3$ toward TA100 without and with S-9mix, respectively. Those toward TA98 were 13,367 and 3,715 revertants/m$^3$, respectively.

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The Experimental Study on the Low-temperature Combustion Characteristics of DME Fuel in a Compression Ignition Engine

  • Yoon, Seung Hyun
    • Journal of ILASS-Korea
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    • v.22 no.4
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    • pp.190-196
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    • 2017
  • The aim of this work is to investigate the combustion and exhaust emission characteristics of low-temperature combustion (LTC) at various EGR test conditions using a single cylinder common-rail diesel engine. In high EGR rate combustion mode with DME fuel, 30% (${\Phi}=0.61$) and 50% (${\Phi}=0.86$) of EGR were respectively examined, and then the combustion, exhaust emissions, nano-particle characteristics of each cases were measured. From these results, it revealed that The ignition delay and combustion duration are prolonged as the increase of EGR rate. In addition, at an advanced injection timing (BTDC $30^{\circ}$), ignition delays were fairly increased because the dilution effect of EGR and also low charge in-cylinder temperature created a lean mixture, thus decreased the peak release rate.

Effect of Sample-loading on Fractionation Efficiency (FE) in a Large Scale Splitter-less Gravitational SPLITT Fractionation (GSF)

  • Lee, Seung-Ho;Lee, Ji-Yeon;Lee, Tae-Woo;Jung, Euo-Chang;Cho, Sung-Kwang
    • Bulletin of the Korean Chemical Society
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    • v.32 no.12
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    • pp.4291-4296
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    • 2011
  • Gravitational SPLITT fractionation (GSF) provides separation of colloidal particles into two subpopulations in a preparative scale. Conventionally, GSF is carried out in a thin rectangular channel having two inlets and two outlets at the top and bottom of the channel, respectively. And the channel is equipped with two flow-splitters, one between the top and bottom inlets and another between the top and bottom outlets. A large scale splitter-less GSF system had been developed, which was designed to operate in the full feed depletion (FFD) mode. In the FFD mode, there is only one inlet through which the sample is fed, thus preventing the sample dilution. In this study, the effect of the sample-loading (in the unit of g/hr) on the fractionation efficiency (FE, number% of particles in a GSF fraction that have the sizes expected by theory) of the new large scale splitter-less FFD-GSF system was investigated. The system was tested in the sample-loading range of 3.0-12.0 g/hr with polyurethane latex beads (PU) and sea-sediment. It was found that there is an optimum range in the sample-loading for a FFD-GSF separation. It was also found that there is a general tendency of FE decreasing as the concentration of the sample suspension increases.

Development and Validation of Primary Method for the Determination of Glucose in Human Serum by Isotope Dilution Liquid Chromatography Tandem Mass Spectrometry and Comparison with Field Methods

  • Lee, Hwa Shim;Lee, Jong Man;Park, Sang Ryoul;Lee, Je Hoon;Kim, Yong Goo
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1698-1702
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    • 2013
  • Glucose is a common medical analyte measuring in human serum or blood samples. The development of a primary method is necessary for the establishment of traceability in measurements. We have developed an isotope dilution liquid chromatography tandem mass spectrometry as a primary method for the measurement of glucose in human serum. Glucose and glucose-$^{13}C_6$ in sample were ionized in ESI negative mode and monitored at mass transfers of m/z 179/89 and 185/92 in MRM, respectively. Glucose was separated on $NH_2P$-50 2D column, and the mobile phase was 20 mM $NH_4OAc$ in 30% acetonitrile/70% water. Verification of this method was performed by the comparison with NIST SRMs. Our results agreed well with the SRM values. We have developed two levels of glucose serum certified reference material using this method and distributed them to the clinical laboratories in Korea as samples for proficiency testings. The expended uncertainty was about 1.2% on 95% confidence level. In proficiency testings, the results obtained from the clinical laboratories showed about 3.6% and 3.9% RSD to the certified values. Primary method can provide the traceability to the field laboratories through proficiency testings or certified reference materials.

Biological Fixation of $CO_2$ by Chlorella sp. HA-1 in a Semi-Continuous and Series Reactor System

  • LEE JAE-YOUNG;KWON TAE-SOON;BAEK KITAE;YANG JI-WON
    • Journal of Microbiology and Biotechnology
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    • v.15 no.3
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    • pp.461-465
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    • 2005
  • Characteristics of biological $CO_2$ fixation by Chlorella sp. HA-1 were investigated in a semi-continuous and series reactor system using an internally illuminated photobioreactor to overcome shortcomings of physicochemical technologies such as adsorption and membrane separation. High $CO_2$ fixation rate was achieved in the semi-continuous reactor system, in which the dilution ratios of the culture medium were controlled. The average $CO_2$ fixation rate was maintained almost constantly when the dilution ratio increased by 0.1 increment from the initial value of 0.5. The total removal efficiency of $CO_2$ was enhanced by employing a series reactor system. The average $CO_2$ fixation rate increased until 4.013 g $CO_2\;day^{-1}$ in a series operation of four reactors, compared to 0.986 g $CO_2\;day^{-1}$ in a batch operation mode. The total $CO_2$ fixation rate was proportional to the number of reactors used in the series reactor system. In the series reactor system of semi-continuous operation, a large amount of $CO_2$ was removed continuously for 30 days. These results showed that the present reactor systems are efficient and economically feasible for a biological $CO_2$ fixation.