• Title/Summary/Keyword: gas chromatographic data

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GC-MS and GC-FID Analysis of Citronella Oil Products for Indicator Ingredient Identification

  • Sumin Kang;Wooil Kim;Jin Wuk Lee;Sangwon Cha
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.160-165
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    • 2023
  • Citronella oil, an essential oil extracted through steam distillation from the leaves and stems of Cymbopogon, is a natural complex substance (NCS) regulated by the Korean government for its use in insect repellents. The component ratios of NCSs like citronella oil vary due to differences in manufacturing processes and origins, presenting a challenge in identifying and quantifying these substances in consumer chemical products. This study analysed ten commercially available products of the most commonly used types of citronella oil, specifically Java and Ceylon types, using gas chromatography (GC)-mass spectrometry (MS) and GC with flame ionization detection (FID). Through chromatographic data, we aimed to determine the components that can qualitatively identify citronella oil and the indicator ingredients that can be used for content analysis.

Rapid Gas Chromatographic Screening of Vegetable Oils for Free Fatty Acids (기체크로마토그래피법에 의한 식물성 유지내 유리 지방산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.373-378
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    • 1993
  • A rapid gas chromatographic profiling method for the simultaneous analysis of free fatty and other acids was applied to vegetable oils. Oil samples were dissolved in dichloromethane and the free acids were extracted with saturated $NaHCO_3$ solution. The aqueous extract was acidified and then loaded onto the Chromosorb P column for the extraction. The acids were eluted with diethyl ether selectively from Chromosorb P column and were treated with triethylamine to prevent the losses of volatile acids. Several long chain fatty acids were detected from soybean oil, rice-bran oil, sesame oil and perilla oil. Various organic acids including odd number fatty acids were detected in crude oil, especially sesame oil. Arachidic acid from perilla oil and vanillic acid from sesame oil, which were not reported before were detected. The content ratio of free linoleic acid to oleic acid was $1.02{\sim}1.18$, which was similar to the reported data. When the GC profile of organic acids were simplified to their corresponding retention index spectra of bar graphical forms, they presented characteristic pattern of each vegetable oil that can be quickly recognized.

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The analysis of Residual Pesticides and Sulfur Dioxide in Commercial Medicinal Plants (유통 한약재의 잔류농약 및 잔류이산화황의 함량 분석)

  • Kim, Tae Hee;Jang, Seol;Lee, Ah Reum;Lee, A Young;Choi, Goya;Kim, Ho Kyung
    • The Korea Journal of Herbology
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    • v.27 no.6
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    • pp.43-48
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    • 2012
  • Objectives : This study was investigated to determine the contents of pesticide residues and sulfur dioxide residues in commercial herbal medicines in Korea. Methods : Chromatographic test was performed on 100 samples consisted with 10 kinds of medicinal plants including improted and domestic products. To establish 19 pesticide residues (DDE, DDD, DDT, Dieldrin, Methoxychlor, BHC isomers, Aldrin, Endosulfan isomers, Endrin, Captan, Procymidone, Chlorpyrifos and Imidacloprid) in commercial herbal medicines, chromatographic equipments were used with the gas chromatography-mass detector and gas chromatography-electron capture detector for qualitative analysis. The imidacloprid analysis was performed by high performance liquid chromatograpgy-ultraviolet detector at 270 nm UV wavelength. The contents of sulfur dioxides were analyzed by modified Monnier-Williams method. All methods were based on notification procedure of Korea Food & Drug Administration (KFDA). Results : The residual pesticides were not founded in improted and domestic samples. Among 100 samples, the residues of sulfur dioxide in 73 samples were not detected and 25 samples showed contents in the range of 0~21.90 mg/kg. The excess samples of MRLs were 2 samples (30 mg/kg to medicinal herbs), Asiasari Radix et Rhizoma (Imported product) and the average amount of sulfur dioxide in 2 unsuitable samples were 14.83 mg/kg. These samples were found to transgress KFDA regulatory guidance of residual sulfur dioxide. Conclusion : These results are able to use as basic data to improve the reliability and value of commercial medicinal herbs.

Study on The System Suitability Test for Alcohols Separation by GCOTC (GCOTC에 의한 알코올류 분리를 위한 시스템 적합성에 관한 연구)

  • Oh, Doe Seok;Kim, Sung Hwa;Lee, Seul;Choi, Jae Gu
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.27 no.2
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    • pp.123-129
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    • 2017
  • Objectives: The purpose of this study is to enhance the application of analytical method of polar solvents(alcohols) by GCOTC (gas chromatography open tubular column) through the system suitability test(SST) to estimate the whole chromatographic system performance(integral part). Methods: To perform the SST, carried out repeatability(n=6) as analytical method of polar solvents by GCOTC, got the retention time($t_R$), standard deviation(${\sigma}_{n-1}$) of $t_R$, baseline width($w_b=4{\sigma}_{n-1}$) and calculated dead time($t_m$) by $v_m=d^2{\pi}L(f/4)$ and $v_m=t_m$ x flow rate. Results: In this experiment, obtained the basic data, there were $t_m=2$ min, methanol($t_R=3.569$, ${\sigma}_{n-1}=0.01$, $w_b=0.04$), ethanol ($t_R=3.892$, ${\sigma}_{n-1}=0.004$, $w_b=0.016$), isopropanol($t_R=4.209$, ${\sigma}_{n-1}=0.004$, $w_b=0.016$). By using these data, calculated the corrected retention time($t_R{^{\prime}}$), capacity factor(k), separation factor(${\alpha}$), number of theoretical plate(n) and resolution($R_s$) for SST and got the good results. Conclusions: Through the SST, could reconfirm the whole chromatographic performance system(integral part) for analytical method of polar solvents by GCOTC. Therefore, this analytical method expect to be widely applied at the related areas.

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.

Urinary Excretion of Triprolidine in Human (인체 뇨에서의 트리프로리딘 배설)

  • 정병화;엄기동;정봉철;박종세
    • Biomolecules & Therapeutics
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    • v.1 no.2
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    • pp.143-150
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    • 1993
  • The metabolic profile of triprolidine, 2-[(4-methylphenyl)-3-(1-pyrrolidinyl-1-propenyl)] pyridine, was determined. Urinary extracts obtained with enzyme hydrolysis were derivatized with MSTFA/TMSCl (N-methyl-N-trimethylsilyl trifluoroacetamide/trimethylchlorosilane) and analyzed by GC/MSD. In human urine, which were obtained after the oral administration with triprolidine, hydroxymethyltriprolidine, triprolidine carboxylic acid, oxotriprolidine carboxylic acid and unchanged triprolidine were detected. The maximum urinary excretion rate of triprolidine and hydroxymethyltriprolidine which were extracted from human urine was at 2 to 4 hours after the drug administration. Triprolidine and hydroxymethyl triprolidine were identified by comparison with authentic standards In chromatographic and mass spectral properties. Triprolidine carboxylic acid was detected as a major metabolite of its metabolites in the urine. Oxotriprolidine carboxylic acid and triprolidine carboxylic acid were tentatively identified by the interpretation of its mass spectral patterns. These data suggest that in human, hydroxylation of either the benzyl or pyrrolidine ring can occur during triprolidine elimination.

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Determination of Ethylene Oxide Rexidue and its Secondary Products in Powdered Food (분말상 식품에 있어서 Enthylene Oxide의 잔류성과 이차생성물 분석)

  • 권중호;김석원;변명우;조한옥;이기동
    • Journal of Food Hygiene and Safety
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    • v.9 no.1
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    • pp.43-48
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    • 1994
  • Instrumental determination was performed for the analysis of residues of ethylene oxide(EO), ethylene chlorohydrin(ECH) and ethylene glycol(EG) in white ginseng powders which were deaerated for 30 min after EO fumigation. Gas chromatographic data showed that EO residues were 570 ppm in the immediate samples after deaeration and 170 ppm in the stored ones for 8 days at 30$\pm$1$^{\circ}C$, respectively, showing a decreasing tendency with elapsed time. On the other hand, ECH and EG residues in samples as the secondary products of EO were 17, 650 ppm and 727 ppm stored for one month, and 9, 595 ppm and 221 ppm stored for 3 months, respectively.

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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.

Reductive Amination of ${\alpha}$,${\beta}$-Unsaturated Carbonyl Compounds with Tetracarbonylhydridoferrate as a Reducing Agent (${\alpha}$,${\beta}$-不飽和 카르보닐化合物의 還元 아미노화反應)

  • Kim Hong-Seok;Shim Sang Chul;Shim Sang Chull
    • Journal of the Korean Chemical Society
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    • v.23 no.2
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    • pp.99-103
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    • 1979
  • The reductive amination of three ${\alpha}$,${\beta}$-unsaturated aldehydes, cinnamaldehyde, crotonaldehyde, and acrolein are carried out successfully by tetracarbonylhydridoferrate in the presence of various primary amines. In a typical reaction, a mixture of potassium tetracarbonylhydridoferrate (22 mmole), an amine (22∼44 mole) and ${\alpha}$,${\beta}$-unsaturated aldehyde (22 mmole), in ethanol (30∼50 ml) was stirred for 9∼60 hours at room temperature under carbon monoxide atmosphere. All the products were characterized as secondary amines by mass, infrared, and nmr spectra as well as gas chromatographic data.

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GC/MS and GC/ECD Analysis of Residual Pesticides in Herbal drugs (GC/MS와 GC/ECD를 이용한 한약재 중 잔류 농약의 분석)

  • Kim, Ho-Kyoung;Park, So-Yeon;Ko, Byoung-Seob
    • The Journal of Korean Medicine
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    • v.20 no.1 s.37
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    • pp.44-51
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    • 1999
  • Analysis of residual pesticides in herbal drugs was performed by GC-ECD and GC-MS. Especially, selected ion monitoring(SIM) technique was applied to increase the GC/MS sensitivity. Analysis of residual pesticides was determined sensitivity and selectively without any internal standard by setting the SIM technique to their characteristic fragments for quantitation ion and confirmation ion. The combination of two detector, GC-ECD and MS-SIM technique, is abailable for determining a multiclass residual pesticides in herbal drugs. The average recoveries through the method were $65.9%{\sim}99.7%$ in herbal drugs. The data of gas chromatographic analysis was compared with the limits of residual pesticides in herbal drugs and agricultural foods. 4. 4-DDT was detected above the limits to the residual pesticides in herbal drugs. Diazinon and EPN were detected, but the limits of residual pesticides were less than that of agricultural foods.

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