• Title/Summary/Keyword: Gas Chromatographic Analysis

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Statistical Analysis of Effective Components for Aroma of Sigumjang

  • Choi, Ung-Kyu;Park, June-Hong
    • Food Science and Biotechnology
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    • v.14 no.2
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    • pp.249-254
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    • 2005
  • The relationship between Sigumjang gas chromatographic patterns precisely analyzed with capillary column and ranked order in sensory analysis was investigated by stepwise multiple regression analysis. Highly predictable multiple regression models were obtained in the analysis. Ninety percent of the Sigumjang aroma was explained by the regression models at step 15 in four transformation except for absolute value transformed with root square and relative value transformed with logarithm. The aroma of Sigumjang was most affected by 2,3-dimethylpyrazine at absolute value and absolute value transformed with logarithm and by 2-furancarboxaldehyde in other transformation. The quality of sigumjang was highly affected by ${\beta}$-phallendrenal, methylpyrazine, tetramethylpyrazine, 5-methyl-2-furancarboxaldehyde, unknown 2, octanoic acid, 4-ethylphenol, methyl 10,13-octadecanoate and ethyl linoleate.

Alternative Sample Preparation Techniques in Gas Chromatographic-Mass Spectrometric Analysis of Urinary Androgenic Steroids

  • Cho, Young-Dae;Choi, Man-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1315-1322
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    • 2006
  • The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.

Analysis of Half-life Time and Residual Concentration of Ethalfluralin Herbicide in Soils (토양 중 제초제 Ethalfluralin의 잔류 농도와 반감기 분석)

  • Han, Seong Soo;Rim, Yo Sup;Kim, Il Kwang
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.168-178
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    • 1997
  • The optimum conditions for the residual analysis of the ethalfluralin herbicide on soils were investigated and the residues in soils were determined by gas chromatography with electron capture detector(GC-ECD). The soil samples extracted with methanol and dichloromethane and concentrated. The concentrated phase were redissolved with toluene and analyzed with GC-ECD after separated by cyanosilica gel Sep-Pak cartridge. From the standard addition experiments with 0.1 and 1.0ppm, the average recoveries were 92.8~101.2% and the detection limit was 0.004ppm. The half-life time of ethalfluralin in the soil(A) was 35 days in the laboratory and 7.2 days in the field test whereas it was 45 days and 9.7 days for each in case of soil(B).

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Simultaneous Analysis of Several Non-Steroidal Anti-Inflammatory Drugs in Urine by Gas Chromatograph/Negative Chemical Ionization-Mass Spectrometry (기체 크로마토그래프-질량분석법을 이용한 뇨중 비스테로이드성 소염진통제 (NSAIDs)의 동시 분석법)

  • Myung, Seung-Woon;Park, Joon-Ho;Kim, Myung-Soo;Cho, Hyun-Woo
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.571-576
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    • 1999
  • Screening method for NSAIDs (Hon-Steroidal Anti-Inflammatory Drugs) in urine was developed using GC/NCI-MS. Derivatized six fenamates with pentafluoropropionic anhydride showed high sensitivity in NCI-MS. The conditions of the derivatization reaction and chromatographic conditions were established for screening with a trace analysis. Limit of detection was in the range of 4-25 pg/mL. This method may be used to the equine doping analysis for NSAIDs and forensic analysis.

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Statistical Analysis on the Sources of Variance in Proficiency Test of Quantitative Analysis of Medicines (의약품 함량분석 정도관리에서의 변이 요인에 대한 통계분석)

  • Cho, Jung-Hwan
    • Journal of Pharmaceutical Investigation
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    • v.37 no.1
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    • pp.27-37
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    • 2007
  • Proficiency test is an essential tool far ensuring analytical ability of analytical chemists and analytical institutes. Usually, the standard protocol for proficiency test is focused on acceptability of reported analytical results of participants by calculating z-scores and related diagnostic parameters. The ultimate goal of this process is to reveal the sources of variability of analytical results and to find the way to reduce their influence. In this study, the method of analysis of variance (ANOVA) was applied to the analytical data collected from qualify control departments of pharmaceutical companies in KyungIn province in Korea in the year of 2000. As influencing factors of variability of analytical results, the use of internal standards for liquid and gas chromatograpy, the educational and professional background of participants, geological locations and yearly production sizes of participating companies were evaluated. To evaluate the variability in accuracy of analytical results, absolute differences from sample mean and sample median were used and to evaluate variability in precision of individual participants, the reported standard deviation of each participant was used. As a result, the use of internal standards in gas chromatographic analysis, participants' academic background and the yearly production sizes of pharmaceutical companies showed statistically significant influence to the accuracy and the precision of the reported analytical results used in this study.

Evaluation of Barley Bran Sauce Aroma by Multiple Regression Analysis

  • Choi, Ung-Kyu
    • Food Science and Biotechnology
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    • v.14 no.5
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    • pp.656-660
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    • 2005
  • The relationship between the gas chromatographic (GC) patterns of sauce made of barley bran and ranked order in sensory analysis was investigated by multiple regression analysis (MRA). Most of the 42 barley bran sauce samples comprised about 34 peaks, in which the content of 9, 12-octadecanoic acid methyl ester was the highest, followed by those of 2-furanmethanol and 2-furancarboxaldehyde. It is difficult to estimate the aroma quality of barley bran sauce samples on the basis of only one peak. The 34 aroma compounds of the 42 samples were analyzed by an MRA model featuring six transformations. The most precise fit was calculated from the absolute value transformed with the root square of each peak, and the multiple determination coefficient showed that 91.6% of the variation in the sensory score could be explained on the basis of GC data.

Studies on Simultaneous Analysis of Organophosphorus Pesticide Residues in Crops by Gas-Liquid Chromatography (I) Extraction and Cleanup (기체-액체 크로마토그래피에 의한 농작물 중 유기인제 잔류 농약의 동시 분석에 관한 연구 (제 1 보). 용매추출 및 방해성분의 분리 제거)

  • Taek-Jae Kim;Yun-Woo Eo;Young Sang Kim
    • Journal of the Korean Chemical Society
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    • v.30 no.5
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    • pp.465-474
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    • 1986
  • The solvent extraction and cleanup processes for the simultaneous gas-liquid chromatographic determination of 11 kinds of organophosphorous pesticide residues in crops were investigated. The extracts dissolved with acetone were partitioned with petroleum ether after adding saturated NaCl solution. Evaporated the partitioning solvent, the residue was dissolved in methylene chloride and eluted through mixed adsorbent (1 : 2 : 4 of activated carbon, magnesia and diatomaceous earth) with methylene chloride as an eluent. The pesticides recovered were 82∼105% and the impurities were effectively removed.

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A Rapid Method for Analysing Polycyclic Aromatic Hydrocarbons (PAH's) in Urban Dust Using Supercritical Fluid Extraction (SFE) and Gas Chromatography/Mass Spectrometry (GC/MS)허귀석, 김달호 (초임계유체추출과 GC/MS를 이용한 도심 대기분진 중 PAH들의 신속한 분석법에 관한 연구)

  • Heo, Gwi Seok;Kim, Dal Ho
    • Journal of the Korean Chemical Society
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    • v.38 no.10
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    • pp.726-733
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    • 1994
  • Supercritical fluid extraction (SFE) followed by gas chromatographic separation and mass spectrometric (MS) detection were used in rapid analysis of polycyclic aromatic hydrocarbons (PAH's) in air particulate material extracted for 30 min with 10 ml of supercritical $N_2O$ without another sample preparation step. Two samples, urban dust in Seoul area and a certified air particulate reference material 1649 supplied by the NBS (National Bureau of Standards), were processed for the purpose of evaluating extraction and analysis methods. As a result, the quantitative recovery of PAH's in the SFE method was relatively lower than conventional organic solvent extraction methods, but reproducibility was resonable, and analysis time was reduced remarkably. The method has proved to be suitable for monitoring of PAH's in air particulate material.

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Comparison between Head Space Gas Sampling and Purge & Trap Sampling in Water Analysis

  • Nagayanagi, Yutaka;Nakagawa, Katsuhiro;Saito, Yoshihiro;Kim, Poongzag
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.739-744
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    • 1995
  • The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

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Studies on Constituents of Higher Fungi of Korea(XL) - A Sterol of Phallus impudicus - (한국산(韓國産) 고등(高等) 균류(菌類)의 성분(成分) 연구(硏究)(제40보)(第40報) - 말뚝버섯의 스테롤 성분(成分) -)

  • Choi, Eung-Chil;Chung, Kyeong-Soo;Kim, Jong-Chan;Kim, Byong-kak
    • The Korean Journal of Mycology
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    • v.11 no.2
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    • pp.97-98
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    • 1983
  • The carpophores of Phallus impudicus collected at Gal-mae-ri in Gyeong-gi Province were subjected to chemical analysis for sterol constituents. The dried carpophores were homogenized and extracted with chloroform-methanol(2 : 1). After saponification of the dried extract, unsaponified components were obtained by ether extraction of the reaction mixture. A sterol fraction was separated by preparative TLC and from this fraction, ergosterol was identified by gas­chromatographic analysis with authentic sterols.

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