• Title/Summary/Keyword: GC method

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QUANTITATION OF BARBITURATES IN URINE BY GC/MS AND ITS COMPARISON TO FLUORESCENCE POLARIZATION IMMUNOASSAY

  • Choo, Hea-Young;Park, Jeongeun;Park, Myung-Ja
    • Toxicological Research
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    • v.7 no.1
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    • pp.29-35
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    • 1991
  • Barbiturates are commonly abused tranquilizer and a rapid method to determine these drugs in biological samples is needed. In this study, was screened barbiturates in urine specimens by the fluorescence polarization immunoassay method(FPIA) and the positive samples were confirmed and identified by the more definitive GC/MS method. Fifteen positive smples which have barbiturate values higher than 0.5 ng/ml were analyzed by the GC/MS method. Eight samples were identified as phenobarbital and five samples were identified as crotilbarbitone.

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The Study on the Composition of Rehmanniae Radix Extracts by Supercritical Carbon Dioxide Extraction and by Hydrodistillation Extraction (생지황(生地黃) 증류 추출 약침액과 초임계 유체 추출물의 성분 연구(硏究))

  • Heo, Jong-Won;Yook, Tae-Han
    • Journal of Acupuncture Research
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    • v.28 no.2
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    • pp.89-95
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    • 2011
  • Objectives : The purpose of this study was to investigate the composition of Rehmannia glutinosa's essential oils with Rehmanniae Radix herbal acupuncture Methods : I obtained the essential oils of Rehmannia Radix by hydrodistillation extraction method and supercritical fluid extraction(SFE) method, and then I analyzed those by GC/MS(gas chromatography/mass spectrum). Results : 1. With GC(gas chromatography) and GC/MS(gas chromatography/mass spectrum) analysis. I identified 9 compounds in the Rehmanniae Radix's essential oil obtained through the SFE method. The main compounds were as follows : Hexachloroethane(2.24%), N-Butyl-benzenesulfonamide(2.05%), hexadecanoic acid(1.93%), hexadecanoic acid, ethyl ester(3.49%), 9,12-Octadecadienoic acid(z,z)(2.70%), (9E)-9-Octadecenoic acid(6.14%), ethyl linoleate(4.43%), ethyl oleate(5.80%). 2. I failed to get Rehmanniae Radix's essential oil obtained through the hydrodistillation method. 3. With GC(gas chromatography) and GC/MS(gas chromatography/mass spectrum) analysis. I identified 4 compounds in the Rehmanniae Radix's essential oil obtained through the hydrodistillation method. The main compounds were as follows : Ethylbis(trimethylsilyl)amine(1.04%), 2-(Trimethylsiloxy)benzoic methyl ester(2.65%), Hexadecanoic acid trimethylsilyl ester(12.61%), octadecanoic acid, trimethylsilyl ester(6.28%). Conclusions : The substances by hydrodistillation method may not perfectly match with the substances by supercritical fluid extraction(SFE) method in essential oils extracted form Rehmanniae Radix. But, the main substances was assumed Hexadecanoic acid and octadecanoic acid.

Analysis of Volatile Compounds in the Gardenia Absoulute Oil (Gardenia Absolute Oil을 구성하고 있는 휘발성 성분의 분석)

  • Ha, Chang-Gyu;Yang, Hae-Ju;Yun, Seok-Sin
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.19 no.1
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    • pp.31-56
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    • 1993
  • The characteristic aroma of Gardenia Absolute Oil made from Gardenia Jasminoides Ellis was investigated by GC and GC-MSD and by sensory evaluation The method of GC Analysis was used Double Column System by Carbowax 20M /SPB-1 of Pola/nonPola columns. And the result data of analysis was checked automatic Relent ion Indexs Match System by GC Workstation. A total of 51 compounds were identified in Gardenia Absolute Oil, including t entatively erstimated 9 compounds. The major components were Linalool, Farnesene of various form, Jasmin Lactone, Gamma undecalactone and Cis-3-hexone derivatives.

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The Stimultaneous Determination of Phenolic Compounds by GC and GC/MS

  • Kim, Jong-Bae;Park, Jyung-Rewng
    • Preventive Nutrition and Food Science
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    • v.3 no.2
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    • pp.111-118
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    • 1998
  • To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.

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Simultaneous Determination of Fructose, Glucose, and Sucrose in Honey and Commercial Drinks by GC and GC/MS (GC 및 GC/MS를 이용한 벌꿀 및 시판 음료 중의 Fructose, Glucose 및 Sucrose의 동시분석)

  • Yun, Jeong-Sik;Jeon, Hyun-Suk;Kim, In-Suk;Lee, Hee-Jin;Lee, Hye-Jeong;Hyun, Jae-Yeoul;Kim, Jong-Bae
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.537-544
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    • 2013
  • This study was performed to establish method of simultaneous determination of fructose, glucose, and sucrose in honey and commercial vitamin drinks by GC and GC/MS. Optimum chromatographic separation of trimethylsilyl-oxime (TMSO) derivatives by GC was achieved on a DB-5 column. Calibration curves for fructose, glucose and sucrose TMSO derivatives by GC were linear in the range of 50-5000 ${\mu}g/mL$, and their $r^2$ values were 0.9999, The limit of detection and limit of quantification of fructose, glucose, and sucrose were 0.68, 0.47, and 0.53 ${\mu}g/mL$, respectively, and 2.27, 1.58, and 1.77 ${\mu}g/mL$, respectively. Average recoveries of fructose, glucose, and sucrose were 100.5, 101.0, and 99.7%, respectively. When the method was applied to 12 honey samples, the average concentrations of fructose, glucose and sucrose were $42.58{\pm}1.97%$, $27.74{\pm}1.16%$, and $0.79{\pm}0.52%$, respectively. The F/G ratio was $1.53{\pm}0.07$. For fructose and glucose contents, results from the GC analysis were similar to those from the HPLC analysis, but the sucrose content was different for each analysis method. We suggest that the GC method is more suitable than other official analytical methods for simultaneous determination of fructose, glucose, and sucrose in honey.

Development of Analytical Method for Picoxystrobin in Agricultural Commodities Using GC/ECD and GC/MS (GC/ECD와 GC/MS를 이용한 농산물 중 Picoxystrobin의 분석법 개발)

  • Kwon, Hye-Young;Kim, Chan-Sup;Park, Byung-Jun;Kim, Il-Hwan;Hong, Su-Myeong;Son, Kyung-Ae;Jin, Yong-Duk;Lee, Je-Bong;Im, Geon-Jae;Kim, Doo-Ho
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.146-151
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    • 2012
  • BACKGROUND: This study was conducted to develop analytical method for picoxystrobin in agricultural commodities using GC/ECD and GC/MS. METHODS AND RESULTS: Each steps of analytical method were optimized for determining picoxystrobin residues in various agricultural commodities. The developed methods include acetone extraction, n-hexane/saline water partition and florisil column chromatography for analysis of all samples (apple, potato, green pepper, hulled rice and soybean), and in addition to these steps, solid phase extraction (SPE) was used for analysis of green pepper and n-hexane/acetonitrile partition was used for analysis of hulled rice and soybean. The instrumental conditions were tested for quantitation in GC/ECD and for confirmation in GC/MS. Recovery was in the range of 86~109% with RSD ${\leq}$10.2% and the quantitation limits (LOQ) of method were 0.025 mg/kg in all agricultural commodities. CONCLUSION: The result showed that the developed method can be used to determine picoxystrobin residue in agricultural commodities.

Development of Analytical Method for Fipronil Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Fipronil의 잔류 분석법 개발)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.309-317
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    • 2015
  • BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.

Comparison of Co-registration Algorithms for TOPS SAR Image (TOPS 모드 SAR 자료의 정합기법 비교분석)

  • Kim, Sang-Wan
    • Korean Journal of Remote Sensing
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    • v.34 no.6_1
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    • pp.1143-1153
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    • 2018
  • For TOPS InSAR processing, high-precision image co-registration is required. We propose an image co-registration method suitable for the TOPS mode by comparing the performance of cross correlation method, the geometric co-registration and the enhanced spectral diversity (ESD) matching algorithm based on the spectral diversity (SD) on the Sentinel-1 TOPS mode image. Using 23 pairs of interferometric pairs generated from 25 Sentinel-1 TOPS images, we applied the cross correlation (CC), geometric correction with only orbit information (GC1), geometric correction combined with iterative cross-correlation (GC2, GC3, GC4), and ESD iteration (ESD_GC, ESD_1, ESD_2). The mean of co-registration errors in azimuth direction by cross correlation and geometric matching are 0.0041 pixels and 0.0016 pixels, respectively. Although the ESD method shows the most accurate result with the error of less than 0.0005 pixels, the error of geometric co-registration is reduced to 0.001 pixels by repetition through additional cross correlation matching between the reference and resampled slave image. The ESD method is not applicable when the coherence of the burst overlap areas is low. Therefore, the geometric co-registration method through iterative processing is a suitable alternative for time series analysis using multiple SAR data or generating interferogram with long time intervals.

Electrochemical Determination of Dopamine Based on Carbon Nanotube-Sol-Gel Titania-Nafion Composite Film Modified Electrode

  • Park, Ji-Ae;Kim, Byung-Kun;Choi, Han-Nim;Lee, Won-Yong
    • Bulletin of the Korean Chemical Society
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    • v.31 no.11
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    • pp.3123-3127
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    • 2010
  • A highly sensitive electrochemical detection method for dopamine (DA) has been developed by relying on a multiwalled carbon nanotube (CNT)-sol-gel titania-Nafion composite film modified glassy carbon (GC) electrode. The CNT-titania-Nafion/GC electrode exhibited excellent electrocatalytic activity towards DA. Therefore, the CNT-titania-Nafion/GC electrode showed improved voltammetric and amperometric responses for DA compared to those obtained with both titania-Nafion/GC and Nafion/GC electrodes. The CNT-titania-Nafion/GC electrode gave a linear response ($R^2$ = 0.999) for DA from $0.5\;{\mu}M$ to 0.5 mM with a detection limit (S/N = 3) of $0.1\;{\mu}M$ and a good sensitivity of 150 mA/M while other electrodes such as CNT-Nafion/GC, titania-Nafion/GC, and a bare GC gave a sensitivity of 89, 39, and 36 mA/M, respectively. Besides, the CNT-titania-Nafion/GC electrode displayed very fast response time within 2 s. The modified electrode showed good selectivity against ascorbic acid. The modified electrode showed good stability and reproducibility. The CNT-titania-Nafion/GC electrode was applied to the determination of DA in urine and serum samples.

Development of an Analytical Method for Chloropicrin Determination in Hulled Rice by GC-ECD and GC-MS (GC-ECD 및 GC-MS를 이용한 현미 중 chloropicrin의 잔류시험법 개발)

  • Do, Jung-Ah;Choi, Jeong-Heui;Park, Hyejin;Park, Yong-Chun;Yoon, Hae-Jung;Choi, Dongmi;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.28 no.3
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    • pp.222-226
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    • 2013
  • A simple and sensitive analytical method was developed using gas chromatograph with electron capture detector (GC-ECD) and gas chromatograph-mass spectrometer (GC-MS) for determination and identification of chloropicrin. Because of small molecular weight and high volatile properties of chloropicrin, analytical method was developed utilizing headspace extraction and direct injection to the GC. The developed method was validated using hulled rice sample spiked with chloropicrin at different concentration levels, 0.1 and 0.5 mg/kg. Average recoveries of chloropicrin (using each concentration three replicates) ranged 77.7~79.3% with relative standard deviations less than 10% and calibration solutions concentration in the range $0.005{\sim}0.5{\mu}g/mL$, and limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The result showed that developed analytical methods was successfully applied to detect a small amount of chloropicrin in hulled rice.