• Title/Summary/Keyword: gas chromatographic analysis

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A rapid separation of Cs, Sr and Ba using gas pressurized extraction chromatography with inductively coupled plasma-mass spectrometry

  • Sojin Jeong;Jihye Kim;Hanul Cho;Hwakyeung Jeong;Byungman Kang;Sang Ho Lim
    • Analytical Science and Technology
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    • v.37 no.2
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    • pp.123-129
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    • 2024
  • We present a rapid method for the determination of Cs, Sr, and Ba, heat generators found in highly active liquid wastes, by gas-pressurized extraction chromatography (GPEC) using a column containing a cation-exchange resin. GPEC is a microscale column chromatographic technique that uses a constant flow rate of solvent (0.07 mL/min) with pressurized nitrogen gas supplied through a valve. In particular, because this method uses a small sample volume (a few hundred microliters), it produces less chemical waste and allows for faster separation compared to traditional column chromatography. In this study, we evaluated the separation of Cs, Sr, and Ba using GPEC. The eluate from the column (GPEC or conventional column chromatography) was quantitatively analyzed using inductively coupled plasma-mass spectrometry to measure the column recovery and precision. The column reproducibility of the proposed GPEC system (RSDs of recoveries) ranged from 2.7 to 4.1 %, and the column recoveries for the three elements ranged from 72 to 98% when aqueous HCl was used as the eluent. The GPEC results are slightly different in efficiency and separation resolution compared to those of conventional column chromatography because of the differences in the eluent flow rate as well as the internal diameter and length of the column. However, the two methods had similar recoveries for Cs and Sr, and the precision of GPEC was improved by two-fold. Remarkably, the solvent volume required for GPEC analysis was five times lower than that of the conventional method, and the total analysis time was 11 times shorter.

Determination of Captan, Folpet, Captafol and Chlorothalonil Residues in Agricultural Commodities using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Captan, Folpet, Captafol 및 Chlorothalonil의 잔류분석법)

  • Lee, Su-Jin;Hwang, Young-Sun;Kim, Young-Hak;Kwon, Chan-Hyeok;Do, Jung-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.29 no.2
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    • pp.165-175
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    • 2010
  • A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.

Optimization of Gas-Liquid Chromatographic Parameters for the Multiresidue Analysis of 24 Pesticides (잔류농약 24성분의 다성분 동시분석을 위한 기체크로마토그래피 조건의 최적화)

  • Lee, Eun-Ju;Kim, Woo-Seong;Park, Kun-Sang;Oh, Jae-Ho;Kim, Dai-Byung
    • The Korean Journal of Pesticide Science
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    • v.4 no.2
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    • pp.11-17
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    • 2000
  • Optimum parameters were investigated for the simultanious analysis of 24 pesticide residuces using gas-liquid chromatography with electron capture detection. Electronic pressure control(EPC) on column enhanced resolution of 24 analyzes. Using DB-17, SPB-608, and Ultra-2 capillary column without EPC incomplete separation was observed in some pairs of pesticides. When EPC function was adopted, no severe overlapping was observed on SPB-608 column in every pesticides except vinclozolin/acetochlor pair. Total running time was 45 min, much shorter than $69{\sim}81$ min when used without EPC. Limit of determination of each analyze ranged $0.1{\sim}12.9$ ng/mL.

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The Screening and Pattern Comparison of Organic Acids in 3 Kinds of Medicinal Herbal Extracts (3가지 약용 허브 추출물에 함유된 유기산 검색 및 조성 비교)

  • Chung, Ha-Yull;Jung, Do-Hyun;Park, Young-Joon
    • Korean Journal of Food Science and Technology
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    • v.32 no.5
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    • pp.997-1001
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    • 2000
  • The organic acids in 3 kinds of medicinal herbal extracts were screened and compared each other according to their organic acid contents by an efficient gas chromatographic method. It involves solid-phase extraction of organic acids using Chromosorb P with subsequent conversion to stable tert-butyldimethysilyl derivatives for the direct analysis by capillary column gas chromatography and gas chromatography-mass spectrometry. Total of 24 organic acids were reproducibly identified from 3 kinds of herbal extracts. When the GC profiles were simplified to their retention index spectra, characteristic patterns were obtained for each herb sample. As expected, three kinds of herbal extracts showed three distinct patterns.

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Analysis of Residual Nuarimol in Apples (사과 중 Nuarimol의 잔류성 분석)

  • Kim, Il Kwang;Han, Seong Soo;Kim, Youn Geun;Kim, Hea Jin
    • Analytical Science and Technology
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    • v.6 no.3
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    • pp.283-288
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    • 1993
  • The solvent extraction and clean up processes for the gas chromatographic determination of muarimol pesticide residues in apples were investigated and examined the changes of residual concentration with the passage of time. The extracted pesticide with methanol were partitioned with dichloromethane after adding sodium chloride solution. The separated solutions were concentrated and transfered to the alumina column for clean up, and eluated with 1-chlorobutane : methanol solution. As a results their recovering for 0.200 and 1.00ppm muarimol spiked on apples have shown 79~95%. Residual amounts of nuarimol in apple was 0.0830ppm when the fungicide was treated eight times until 3 days before its harvest. It seems to be safely used when nuarimol is treated six times until 7 days before harvest of apple.

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Calibration Methods for the Gas Chromatographic Analysis of ppt-level Hydrogen Sulfide (H2) in Air (환경 대기 중 ppt 수준의 황화수소 분석을 위한 GC 방식의 검량 기법에 대한 연구)

  • 김기현;오상인;최여진;최규훈;주도원
    • Journal of Korean Society for Atmospheric Environment
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    • v.19 no.6
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    • pp.679-687
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    • 2003
  • In this study, we investigated the analytical techniques to quantify the ambient concentration of hydrogen sulfide (H$_2$S) in air at ppt concentration level. For this purpose, an on-line GC analytical system equipped with both pulsed-flame photometric detector (PFPD) and thermal desorption unit (TDU) was investigated by collecting ambient air samples. The results of our study generally indicated that calibration conditions of GC system is highly sensitive to affect the accuracy of the analytical technique. Most importantly. we found that the use of different matrices in the the preparation stage of working standards was sensitive to control the overall performance of this technique. The calibration of our analytical system was tested by the two types of working standard (prepared by mixing either with high purity $N_2$ or with the ambient air). According to this test, the latter represented more efficiently the detecting conditions of actual air samples. The peak occurrence patterns of both air samples and standards (prepared by mixing with ambient air) were altered in a similar manner as the function of the loaded volume; however, it was not the case for the $N_2$-mixed standards. Results of our study suggest that detection of H$_2$S is highly different from other sulfides and that its quantification requires minimiaing interfering effects of non -pure substance (like water vapor) and (either sorptive or destructive) loss effects.

VOLATILE CONSTITUENTS OF COOKED SQUID (피등어꼴뚜기의 자숙취에 관한 연구)

  • LEE Eung-Ho;KOIZUMI Chiaki;NONAKA Junsaku
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.11 no.4
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    • pp.183-188
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    • 1978
  • In this study, gas chromatographic analysis was carried out on volatile constituents of cooked squid for the object of obtaining information on the characteristic flavor of the cooked squid meat. The results obtained are as follows: 1) Methanol was the most effective solvent for the extraction of volatile constituents of squid meat. 2) Twenty five and thirty two peaks were detected from the condensate collected in cold traps which were immersed in ice water and dry ice-acetone, respectively. In these compounds, five kinds of volatile organic acids such as acetic acid, butyric acid, iso-valeric acid, valeric acid, and caproic acid were identified. 3) Eleven peaks were detected from the head space vapor collected in cold trap which is immersed in liquid nitrogen. Volatile amines identified in these components are as follows; methylamine, trimethylamine, dimethylamine, ethylamine, and iso-propylamine.

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Studies on the Sterol of Sesame Oil Sold In Markets and Used in Restaurants (시중(市中) 참기름의 Sterol에 관(關)한 연구(硏究))

  • Ro, Ihl-Yeob;Jeong, Hee-Sun
    • Journal of Nutrition and Health
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    • v.13 no.4
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    • pp.159-166
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    • 1980
  • Methods for the determination of sterols in sesame oils were studied. The sesame oils were saponified and the sterols isolated from the unsaponifiable matter by Florisil column chromatography, and the individual components were determined by means of gas chromatography. Campesterol, ${\beta}-sitosterol$, stigmasterol were found in sesame oil including unknown Ⅰ and Ⅱ. The use of SE-30 gas chromatographic column allows the slow elution, duplication of peaks and relatively low reproducibility, therefore, 3% OV-17 was suitable for the sterol analysis. The result of this study showed that contents of sterols in sesame oil were campesterol 8.4%, stigmasterol 4.5%, ${\beta}-sitosterol$ 33.9% and others 53.0% involving 8.8% of unknown I and 44.3% of unknown Ⅱ. There has been no specific test available for identifying the sesame oil among common edible oils. But the ratio of sterols in sesame oils allowed the estimation of genuiness. The ratio of sterols vs. campesterol in genuine sesame oils were stigmasterol 0.3- 0.6, ${\beta}-sitosterol$ 3.0-3.8 and unknown Ⅱ 3.0, respectively. The 65 samples were composed of genuine sesame oil 40%, mixed rape seed oil 3%, cotton seed oil 1. 5% others were reused soybean oil or re-extracted oil.

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Aspergillus clavatus Y2H0002 as a New Endophytic Fungal Strain Producing Gibberellins Isolated from Nymphoides peltata in Fresh Water

  • You, Young-Hyun;Kwak, Tae Won;Kang, Sang-Mo;Lee, Myung-Chul;Kim, Jong-Guk
    • Mycobiology
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    • v.43 no.1
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    • pp.87-91
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    • 2015
  • Eighteen endophytic fungi with different colony morphologies were isolated from the roots of Nymphoides peltata growing in the Dalsung wetland. The fungal culture filtrates of the endophytic fungi were treated to Waito-c rice seedling to evaluate their plant growth-promoting activities. Culture filtrate of Y2H0002 fungal strain promoted the growth of the Waito-c rice seedlings. This strain was identified on the basis of sequences of the partial internal transcribed spacer region and the partial beta-tubulin gene. Upon chromatographic analysis of the culture filtrate of Y2H0002 strain, the gibberellins (GAs: $GA_1$, $GA_3$, and $GA_4$) were detected and quantified. Molecular and morphological studies identified the Y2H0002 strain as belonging to Aspergillus clavatus. These results indicated that A. clavatus improves the growth of plants and produces various GAs, and may participate in the growth of plants under diverse environmental conditions.

Studies on the Oil Soluble Constituents of Korean Ginseng -Part 1. On the Composition of Ginseng Sterols- (한국인삼(韓國人蔘)의 유용성성분(油溶性成分)에 관한 연구(硏究) -제1보 Sterol 성분(成分)에 관하여-)

  • Ko, Young-Su
    • Korean Journal of Food Science and Technology
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    • v.8 no.4
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    • pp.201-206
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    • 1976
  • Korean ginseng sterols were obtained from the non-saponifiable matters of etherial extract of the root. The composition of sterols have been determined by gas liquid chromatography and thin-layer chromatographic analysis. The results showed that contents of sterols were ${\beta}-sitosterol$, 77.87% by method of triangulation and 82.72% by methode of planimetry and stigmasterol,15.39% by methode of triangulation and 13.92% by methode of planimetry and campesterol, 6.74% by method of triangulation and 4.36% by methode of planimetry.

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