• 제목/요약/키워드: gas-liquid chromatography

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Analytical Method for Dioxin and Organo-Chlorinated Compounds : (I) Pretreatment of Milk Samples for Dioxin Analysis

  • 양정수;김진영;최용욱;이대운
    • Bulletin of the Korean Chemical Society
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    • v.19 no.6
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    • pp.619-624
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBS) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Qualitative Analysis of the Major Constituents in Traditional Oriental Prescription Bang-poong-tong-sung-san by Liquid Chromatography/Ultraviolet Detector/Ion-Trap Time-of-Flight Mass Spectrometry

  • Eom, Han Young;Kim, Hyung-Seung;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.24-29
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    • 2014
  • An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

Development of Simultaneous Analysis for the Multi-residual Pesticides in the Ginseng Extract using Gas Chromatography (인삼농축액에서 GC를 이용한 잔류농약 동시다성분 분석법의 개발)

  • Shin Yeong-Min;Lee Seon-Hwa;Son Yeong-Uk;Jeong Ji-Yoon;Jeoung Seoung-Wook;Park Heung-Jai;Kim Sung-Hun;Won Young-Jun;Lee Chang-Hee;Kim Woo-Seong;Hong Moo-Ki;Chae Kab-Ryong
    • Journal of Environmental Science International
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    • v.15 no.1
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    • pp.85-94
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    • 2006
  • The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

A Study on the Research of Analytical Method for 1,4-Dioxane in Water (1,4-Dioxane의 분석방법 연구)

  • Park, Sun-Ku;Kim, Tae-Ho;Rim, Yeon-taek;Myung, Nho-Il
    • Journal of Korean Society on Water Environment
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    • v.21 no.6
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    • pp.549-563
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    • 2005
  • The study was carried out to develop and standardize the analytical method of 1,4-dioxane in water. The National Institute of Environmental Research in Korea has monitored for 1,4-dioxane in water since 1998 and it has been detected in environmental water occasionally. But the environmental pollution and analytical method in water is not well known over the world. The trace analytical method at low-${\mu}/L$ level is prerequisite in order to evaluate the residue of 1,4-dioxane in water. Evaluation of the method was demonstrated by comparing and analyzing with liquid-liquid extraction, solid-phase extraction and purge & trap technique. As a result of experiment by standard solutions and raw samples, the precision and accuracy for three methods were obtained within error rate of about 10%. Therefore, three methods were standardized as official monitoring method in Korea. Also, a convenient and simple liquid-liquid extraction method for the analysis of 1,4-dioxane in water was developed by combined with gas chromatography/mass spectrometry and applied to the water samples in Korea

Quantitative Determination of Styrene in Blood and Mandelic Acid in Urine of the Occupationally Styrene-exposed Workers

  • Yang, Jeong-Sun
    • Archives of Pharmacal Research
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    • v.17 no.2
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    • pp.76-79
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    • 1994
  • The concentration of styrne in blood of the occupationally syrene-exposed workers was checked by gas chromatographic headspace analysis. Mandelic acd in urine, that is a major metabolite of styrene, and hippuric acid wre also analyzed by high performance liquid chromatography. For the biological monitoring of styrene-exposed workers, the routine method of the quantitative determination of styrene nad its metabolites in the biolgical samples were studied.

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Characteristic Analysis of GTL Fuel as an Automobile Diesel (자동차용 경유로서 GTL의 연료특성분석)

  • Lim, Young-Kwan;Shin, Seong-Cheol;Kim, Jong-Ryeol;Yim, Eui-Soon;Song, Hung-Og;Kim, Dongkil
    • Applied Chemistry for Engineering
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    • v.19 no.6
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    • pp.617-623
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    • 2008
  • GTL (gas-to-liquid) fuel produced by the Fischer-Tropsch reaction of carbon monoxide (CO) and hydrogen ($H_2$) is expected to be one of the environmental friendly biomass based alternatives and blended to petrodiesel. In this study, the characteristic of the fuel was analyzed by its concentration differences after blending petrodiesel in domestic market with different amounts of GTL fuel which produced from Shell. Gas chromatography shows that GTL fuel consists of longer paraffin chain than common diesel. GTL fuel showed a high flash point, distillation, kinematic viscosity, and derived cetane number. In addition, GTL fuel showed lower lubricity due to low sulfur content.

Development of power system and degradation technology using arc plasma for the degradation of non degradable waste water (플라즈마를 이용한 액상 폐기물 처리 전원장치 개발 및 분해 기술 개발)

  • Han, Chul-Woo;Kim, June-Sung;Park, Sang-Hoon;Hwang, Lee-Ho;Rhee, Byong-Ho;Kang, Duk-Won;Kim, Jin-Kil
    • Proceedings of the KIEE Conference
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    • 2004.07c
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    • pp.1900-1902
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    • 2004
  • The degradation systems of non degradable waste water consist of the arc plasma torch, power supply, a feeder of liquid waste and reactors. Output of stable plasma torch, suitable air flux, microscopic atomizing state of waste water and long reaction section must be to degrade waste water more efficiently. In this paper, we are designed the stable power system, the microscopic atomizing state of waste water and the efficient reactors to satisfy various conditions. Non degradable wast water used in this work was $Na_2$EDTA of 1.0 mol. The concentration of $CO_2$ and EDTA was analyzed using GC (Gas Chromatography) and HPLC (High Performance Liquid Chromatography). In the result show that $CO_2$ concentration was about 96% and EDTA was degraded approximately 96%.

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Studies on the Composition of Green and Roast Coffee bean (커피생두(生豆)(Green Coffee)와 볶은 커피두(豆)(Roast Coffee)의 성분(成分)에 관(關)한 연구(硏究))

  • Choi, Min-Kang;Lee, Yong-Ock;Ko, Young-Su
    • Journal of Nutrition and Health
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    • v.11 no.1
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    • pp.9-16
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    • 1978
  • A Comparison of the analysis of the green and roast coffee of Arabica and Robusta compositions and regular instant coffee has been investigated by chromatography. The coffee oil were obtained by extracting the green and roast coffee with ethyl ether by soxhlet methood. Instant coffee samples were accurately weighted into 100ml beaker (ca. 0.5g regular coffee and 1.5g decaffeinated coffee) and add ca. 50ml water, heat and boil, remove from heat, and mechanically stried ca. 15min. and filtered of one sample and another sample were without filtrated and proceed with liquid chromatographic separation. The fatty acid compositions of green and roast coffee were compared by gas liquid chromatography and general chemical compositions of sample were analysed. Some similarities between green and roast coffee fatty acids were found in the case of green and roast coffee of both kinds acid methyl esters. They contained stearic, oleic, linoleic, and unknown fatty acid, and palmitic ana linoleic acid were rich.

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A Study on the Separation and Extraction of Polycyclic Aromatic Hydrocarbons in Water Sample by Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법에 의한 물시료 중 Polycyclic Aromatic Hydrocarbons의 분리 및 추출에 관한 연구)

  • Lee, Won;Hong, Jee-Eun;Park, Song-Ja;Pyo, Hee Soo;Kim, In-Whan
    • Analytical Science and Technology
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    • v.11 no.5
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    • pp.321-331
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    • 1998
  • The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAHs) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some extraction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAHs was possible by partial variation of oven temperature of GC/MS in temperature range $80{\sim}310^{\circ}C$. Extraction procedures of PAHs in water samples were somewhat modified and compared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAHs were 71.3~109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7~94.9%) were obtained in case of $C_{18}$ disk extraction method by filtration. And extraction recoveries of PAHs by $C_{18}$ solid-phase were in the range of 51.8~77.9%. Method detection limits (S/N=5) of 19 PAHs were in the range of 0.25~6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05~1.25 ppb by disk extraction methods.

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Analysis of Trans Fat in Edible Oils with Cooking Process

  • Song, Juhee;Park, Joohyeok;Jung, Jinyeong;Lee, Chankyu;Gim, Seo Yeoung;Ka, HyeJung;Yi, BoRa;Kim, Mi-Ja;Kim, Cho-il;Lee, JaeHwan
    • Toxicological Research
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    • v.31 no.3
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    • pp.307-312
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    • 2015
  • Trans fat is a unsaturated fatty acid with trans configuration and separated double bonds. Analytical methods have been introduced to analyze trans fat content in foods including infrared (IR) spectroscopy, gas chromatography (GC), Fourier transform-infrared (FT-IR) spectroscopy, reverses-phase silver ion high performance liquid chromatography, and silver nitrate thin layer chromatography. Currently, FT-IR spectroscopy and GC are mostly used methods. Trans fat content in 6 vegetable oils were analyzed and processing effects including baking, stir-frying, pan-frying, and frying on the formation of trans fat in corn oil was evaluated by GC. Among tested vegetable oils, corn oil has 0.25 g trans fat/100 g, whereas other oils including rapeseed, soybean, olive, perilla, and sesame oils did not have detectable amount of trans fat content. Among cooking methods, stir-frying increased trans fat in corn oil whereas baking, pan-frying, and frying procedures did not make changes in trans fat content compared to untreated corn oils. However, the trans fat content was so low and food label can be declared as '0' trans based on the regulation of Ministry of Food ad Drug Safety (MFDS) (< 2 g/100 g edible oil).