• Title/Summary/Keyword: capillary column

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Development of Analytical Method for Propylene Glycol in Foods (식품 중 프로필렌글리콜의 분석법 개발)

  • Kim, Hee-Yun;Hong, Ki-Hyoung;Choi, Jang-Duck;Park, Sung-Kwan;Jung, Si-Sub;Choi, Woo-Jeong;Lee, Shin-Ho;Moon, Dong-Chul
    • Korean Journal of Food Science and Technology
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    • v.37 no.6
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    • pp.889-892
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    • 2005
  • Standardized method based on extraction, filtration, and gas chromatography (GC) was developed far propylene glycol analysis to set hygienic norm of safety measure for foods under governmental control. Various columns were tested fur propylene glycol analysis by GC with flame ionization detector. Known amount of propylene glycol was spiked into wheat flour dough and analyzed by developed method. Results showed 101.60% recovery rate for propylene glycol with HP-5 column. Reproducibility test of standards recorded 0.30 for standard variation and 0,42% for relative variation. Using analytical method established, contents of propylene glycol in more than hundred different foods were monitored. Propylene glycol was detected in most foods, indicating propylene glycol is not only commonly added during food preparation, but also is contained naturally in food.

Adsorption and Transfer of Trace Elements in Repellent Soils (토양 소수성에 따른 미량원소의 흡착 및 이동)

  • Choi, Jun-Yong;Lee, Sang-Soo;Ok, Yong-Sik;Chun, So-Ul;Joo, Young-Kyoo
    • Korean Journal of Soil Science and Fertilizer
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    • v.45 no.2
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    • pp.204-208
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    • 2012
  • Water repellency which affects infiltration, evaporation, erosion and other water transfer mechanisms through soil has been observed under several natural conditions. Water repellency is thought to be caused by hydrophobic organic compounds, which are present as coatings on soil particles or as an interstitial matter between soil particles. This study was conducted to evaluate the characteristics of the water repellent soil and transport characteristics of trace elements within this soil. Capillary height of the water repellent soil was measured. Batch and column studies were accompanied to identify sorption and transport mechanism of trace elements such as $Cu^{2+}$, $Mn^{2+}$, $Fe^{2+}$, $Zn^{2+}$ and $Mo^{5+}$. Difference of sorption capacity between common and repellent soils was observed depended on the degree of repellency. In the column study, the desorption of trace elements and the spatial concentration distribution as a function of time were evaluated. The capillary height was in the repellency order of 0% > 15% > 40% > 70% > 100%. No water was absorbed in soil indicating >70% repellency. Using trace elements, $Fe^{2+}$ and $Mo^{5+}$ showed higher sorption capacity in the repellent soil than in non-repellent soil. The sorption performance of $Fe^{2+}$ was found to be in the repellency order of 40% > 15% > 0%. Our results found that transfer of $Mo^{5+}$ had similar sorption tendency in soils having 0%, 15% and 40% repellency at the beginning, however, the higher desorption capacity was observed as time passes in the repellent soil compared to in non-repellent soils.

Trans Fatty Acid Isomers of Processed Foods Commonly Consumed in Korea (한국인 상용 가공식품의 trans 지방산 이성체)

  • 노경희;원미숙;송영선
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.3
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    • pp.325-337
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    • 2003
  • This study was designed to determine the distribution of trans fatty acids (tFAs) isomers of Processed foods commonly consumed in Korea. The tFAs positional isomers were analyzed using GC/MS spectrometer with HP-23 cis/trans FAME, capillary column (50m $\times$ 0.20 mm, id., 0.2 ${\mu}{\textrm}{m}$ film thickness) for 41 food samples. TFAs isomers were identified by comparing retention time with standards and GC/MS spectrum. In margarines, the content of tFAs ranged from 4.0% to 25.16% and the most abundant positional isomer of tFAs was C18:1 $\Delta$9t. In oils and fats, lards contained higher levels of tFAs (5.70~16.54%) than shortenings (6.77~10.55%). Shortenings contained higher levels of C18:1 $\Delta$9t (3.1~5.1%) than lard (1.6~4.3%), but corn oils had no tFAs. In seasonings, mayonnaise had no C16:1 $\Delta$9t, whereas C18:3t was detected. The content of tFAs in confectioneries was wide (16.20~52.16%). Among them, instant popcorns contained the highest amount of tFAs. Milk and dairy products showed even distribution of tFAS such as C18:1t, C18:2t, and C18:3t. Predominant tFAS isomer of condensed milk and ice cream was C16:1 $\Delta$9t. Frozen french fries and fried chicken contained higher levels of C18:1$\Delta$9t (9.4%), whereas grilled pork (jowl) had no C18:1 $\Delta$9t. The amount of tFAs per serving size was the highest in popcorn, followed by frozen pizza, frozen french fries, fried chicken, and bakeries.

Evaluation of Hydrogeologic Seal Capacity of Mudstone in the Yeongil Group, Pohang Basin, Korea: Focusing on Mercury Intrusion Capillary Pressure Analysis (포항분지 영일층군 이암층의 수리지질학적 차폐능 평가: 수은 모세관 압입 시험의 결과 분석을 중심으로)

  • Kim, Seon-Ok;Wang, Sookyun;Lee, Minhee
    • Economic and Environmental Geology
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    • v.53 no.1
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    • pp.23-32
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    • 2020
  • Geological CO2 sequestration is a global warming response technology to limit atmospheric emissions by injecting CO2 captured on a large scale into deep geological formations. The presented results concern mineralogical and hydrogeological investigations (FE-SEM, XRD, XRF, and MICP) of mudstone samples from drilling cores of the Pohang basin, which is the research area for the first demonstration-scale CO2 storage project in Korea. They aim to identify the mineral properties of the mudstone constituting the caprock and to quantitatively evaluate the hydrogeologic sealing capacity that directly affects the stability and reliability of geological CO2 storage. Mineralogical analysis showed that the mudstone samples are mainly composed of quartz, K-feldspar, plagioclase and a small amount of pyrite, calcite, clay minerals, etc. Mercury intrusion capillary pressure analysis also showed that the samples generally had uniform particle configurations and pore distribution and there was no distinct correlation between the estimated porosity and air permeability. The allowable CO2 column heights based on the estimated pore-entry pressures and breakthrough pressures were found to be significantly higher than the thickness of the targeting CO2 injection layer. These results showed that the mudstone layers in the Yeongil group, Pohang basin, Korea have sufficient sealing capacity to suppress the leakage of CO2 injected during the demonstration-scale CO2 storage project. It should be noticed, however, that the applicability of results and analyses in this study is limited by the lack of available samples. For rigorous assessment of the sealing efficiency for geological CO2 storage operations, significant efforts on collection and multi-aspect evaluation for core samples over entire caprock formations should be accompanied.

Isolation of Isoflavones and Soyasaponins from the Germ of Soybean (콩 배아로 부터 Isoflavone과 Soyasaponin의 동시 분리)

  • Kim, Sun-Lim;Lee, Jae-Eun;Kim, Yul-Ho;Jung, Gun-Ho;Kim, Dea-Wook;Lee, Choon-Ki;Kim, Mi-Jung;Kim, Jung-Tae;Lee, Yu-Young;Hwang, Tae-Young;Lee, Kwang-Sik;Kim, Wook-Han;Kwon, Young-Up;Kim, Hong-Sig;Chung, Ill-Min
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.58 no.2
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    • pp.149-160
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    • 2013
  • The objective of present study was to simultaneously isolate of isoflavone and soyasaponin compounds from the germ of soybean seeds. Soy germ flours were defatted with hexane for 48h at room temperature, and methanolic extracts were prepared using reflux apparatus at $90^{\circ}C$ for 6h, two times. After extraction, extracts were separated with preparative RP-$C_{18}$ packing column ($125{\AA}$, $55-105{\mu}m$, $40{\times}150mm$), and collected 52 fractions were identified with TLC plate (Kieselgel 60 F-254) and HPLC, respectively. Among the identified isoflavone and soyasaponin fractions, isoflavone fractions were re-separated using a recycling HPLC with gel permeation column (Jaigel-W252, $20{\times}500mm$). Final fractions were air-dried, and the purified compounds of two isoflavones (ISF-1-1, ISF-1-2) and four soyasaponins (SAP-1, SAP-2, SAP-3, SAP-4) were obtained. Two isoflavone compounds (ISF-1-1, ISF-1-2) were acid-hydrolyzed for the identification of their aglycones, and confirmed by comparing with 12 types of isoflavone isomers. While the four kinds of soyasaponins were identified by using a micro Q-TOF mass spectrometer in the ESI positive mode with capillary voltage of 4.5kV, and dry temperature of $200^{\circ}C$. Base on the obtained results, it was conclude that ISF-1-1 is the mixture isomers of daidzin (43.4%), glycitin (47.0%), and genistin (9.6%), but ISF-1-2 is the single compound of genistin (99.8% <). On the other hand, soyasaponin SAP-1 is the mixture compounds of soyasaponin A-group (Aa, Ab, Ac, Ae, Af); SAP-2 is soyasaponin B-group (Ba, Bb, Bc) and E-group (Bd, Be); SAP-3 is soyasaponin B-group (Ba, Bb, Bc), E-group (Bd, Be), and DDMP-group (${\beta}g$); SAP-4 is soyasaponin B-group (Ba, Bb, Bc), E-group (Bd, Be), and DDMP-group (${\beta}g$, ${\beta}a$), respectively.

Simultaneous Determination of Cholesterol, Bile Acids and Sterols in Human Bile Juices and Gallstones Using GC/MS (GC/MS에 의한 담석과 담즙내의 Cholesterol, Bile Acids 및 Sterols의 동시 Profiling)

  • Yang, Yoon Jung;Lee, Seon Hwa;Kim, Hyun Joo;Chung, Bong Chul
    • Journal of the Korean Chemical Society
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    • v.42 no.3
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    • pp.266-276
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    • 1998
  • Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

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Separation of Chromophoric Substance from Amur Cork Tree Using GC-MS (GC-MS를 이용한 황벽의 색소 성분 분리 거동)

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.33 no.6
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    • pp.980-989
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    • 2009
  • Amur cork tree was extracted in methanol with the purpose of investigating the most effective extraction procedure for detecting the chromophore using the GC-MS analysis. Different procedures of waterbath and hotplate extractions were carried out and five different GC-MS instrument parameters including the operating temperatures in the GC capillary column and the MSD scan range were tested for their efficiencies. Berberine was determined by the detection of dihydroberberine at 15.0 min r.t. Hotplate was a better device for extracting amur cork tree than waterbath shaker either with or without presoaking in the room temperature. Water was not an adequate extraction medium for the berberine detection. The most effective GC-MS parameter was Method 4; the initial temperature at $50^{\circ}C$ followed by the temperature increase of $23^{\circ}C$/min until $210^{\circ}C$, then increase of $30^{\circ}C$/min until the final temperature reach at $305^{\circ}C$, then hold for 14 minutes to maintain the total run time 24.12 minutes. The MSD scan range for Method 4 was $35\sim400$m/z.

Optimization of Soybean Oil Fatty Acid Methyl Esters Preparation for Sucrose Polyesters Synthesis (Sucrose polyesters 합성에 사용하는 대두유 지방산 메틸에스테르 제조의 최적화)

  • Chung, Ha-Yull;Kim, Suk-Ju;Yoon, Sung-Woo;Yoon, Hee-Nam;Kong, Un-Young
    • Korean Journal of Food Science and Technology
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    • v.24 no.3
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    • pp.240-246
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    • 1992
  • Preparation of soybean oil fatty acid methyl esters (soybean oil FAME) through the transesterification of soybean oil with alkaline catalyst was optimized in terms of contents of residual free fatty acids (FFA) in soybean oil FAME and yield of soybean oil FAME due to the inhibitory effect of FFA on sucrose polyesters synthesis. Soybean oil FAME and residual FFA were analyzed quantitatively by simultaneous gas chromatography on a fused silica capillary column after converting the FFA in soybean oil FAME to tert.-butyldimethylsilyl (TBDMS) derivatives. Transesterification of soybean oil was successfully performed with alkaline catalyst (NaOH, 95%), which resulted in 99.1% yield of soybean oil FAME and less than 0.1% residual FFA contents under the conditions such as $30^{\circ}C$, 20min. and 6:1 molar ratio of anhydrous methanol to soybean oil.

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Solvent-free determination of BTEX in water using repetitive membrane extraction followed by GC-MS (반복적인 막 추출과 GC-MS를 이용한 물 중 BTEX의 분석)

  • Kim, He-Kap;Kim, Se-Young;Lee, Soo-Hyung
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.352-359
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    • 2011
  • An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap ($-100^{\circ}C$) with helium gas. The BTEX compounds, thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at $20{\pm}2^{\circ}C$. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%) with good-linearity calibration curves ($r^2$ 0.9976-0.9997 in 1-100 ${\mu}g$/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 ${\mu}g$/L. The results showed the method's advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.

Analysis of some pesticides in urine by GC/MS (GC/MS를 이용한 뇨중 몇가지 농약의 분석)

  • Park, Seong-Soo;Park, Song-Ja;Pyo, Hee-Soo;Cho, Jung-Hee;Kim, Hye-Soo;Park, Taek-Kyu
    • The Korean Journal of Pesticide Science
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    • v.4 no.1
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    • pp.1-10
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    • 2000
  • The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

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