• Title/Summary/Keyword: (GC-MS) gas chromatography-mass spectrometry analysis

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Quantitative and Comparative Analysis of Urinary Steroid Levels upon Treatment of an Anti-Diabetic Drug, CKD-501 using Gas Chromatography-Mass Spectrometry

  • Sadanala, Krishna Chaitanya;Jung, Byung-Hwa;Jang, In-Jin;Chung, Bong-Chul
    • Journal of Pharmaceutical Investigation
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    • v.41 no.1
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    • pp.37-43
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    • 2011
  • Urinary steroid levels were investigated in the treatment of CKD-501, a new anti-diabetic drug candidate. CKD-501 was administered orally at the dosage of 1, 2, 4 mg/day for 7 days to normal men (n=18). Urine was collected before, during and after stopping the drug administration and the urinary level of androgen, estrogen, progestin and corticoids were quantified using GC-MS (gas chromatography-mass spectrometry). Only urinary corticosteroid and an androgen, DHEA levels among all the analyzed steroids, have been found to increase progressively, reaching significant levels on the last day of drug treatment and later declined after the drug treatment is withdrawn. Therefore, it was thought that an increase in the urinary corticoid and DHEA levels could be a characteristic of CKD-501, since it prominently acts on the glucose sensitivity and suppresses the triglyceride levels. In conclusion, it was found that CKD-501, an anti-diabetic drug candidate, affects the glucocorticoid and DHEA levels and it plays a crucial role in glucose homeostasis.

Protective Effect of Water Extract of Fraxinus Rhynchophylla Leaves on Acetaminophen-induced Nephrotoxicity in Mice and Its Phenolic Compounds

  • Jeon, Jeong-Ryae;Choi, Joon-Hyuk
    • Food Science and Biotechnology
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    • v.16 no.6
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    • pp.988-993
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    • 2007
  • The protective effect of the water extract of Fraxinus rhynchophylla leaves (FLE) was determined using an animal model of acetaminophen (AAP)-induced nephrotoxicity. The BALB/c male mice used in this study were divided into 3 groups; the normal, AAP-administered, and FLE-pretreated AAP groups. A single dose of AAP induced necrosis of renal tubules and congestion along with edema to a remarkable degree as observed by hematoxylin and eosin stain, and also increased the numbers of terminal deoxynucleotidyl transferase-mediated deoxyuridine triphosphate nick end labeling (TUNEL)-positive renal tubular epithelial cells. Blood urea nitrogen and plasma creatinine levels were determined to be significantly higher in the AAP group than in the normal group. However, FLE pretreatment resulted in an attenuation of renal tubule necrosis. Regeneration and dilatation of renal tubules were noted, and the numbers of TUNEL-positive cells were reduced in the FLE-pretreated groups. In an effort to detect the bioactive compounds exerting protective effects in FLE, the analysis of phenolic compounds via gas chromatography/mass spectrometry (GC/MS) were performed, and identified esculetin and esculin. The present study indicates that these compounds may exert a protective effect against AAP-induced nephrotoxicity.

Quantitative Analysis of Isoflavones and Lignans in Sea Vegetables Consumed in Korea Using Isotope Dilution Gas Chromatography-Mass Spectrometry

  • Lee, Young-Joo;Adlercreutz, Herman;Kwon, Hoon-Jeong
    • Food Science and Biotechnology
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    • v.15 no.1
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    • pp.102-106
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    • 2006
  • The phytoestrogens including isoflavones (genistein, daidzein, biochanin A, formononetin, and glycitein), coumestrol, and lignans (secoisolariciresinol, matairesinol, and anhydrosecoisolariciresinol) were quantified in edible sea vegetables from Korea. Sea vegetable samples were collected based on domestic consumption data. After hydrolysis of phytoestrogen glycosides in prepared samples, aglycones of phytoestrogens were extracted with diethyl ether and analyzed with isotope dilution gas chromatography-mass spectrometry in selected ion monitoring mode (ID-GC-MS-SIM). Total samples included 19 samples representing eight species. Most of the samples showed rather low concentrations, ranging from not determinated to $79.2\;{\mu}g/kg$ for isoflavones and from 106.4 to $694.8\;{\mu}g/kg$ for lignans. The daily intake of phytoestrogen from sea vegetables, estimated from the present data and domestic consumption data, was about $0.13\;{\mu}g/day$ for isoflavones and $2.0\;{\mu}g/day$ for lignans. When we compared these results with those from legumes, sea vegetables would not be considered the major source of phytoestrogens in the Korean diet.

Evaporation Characteristics of Oil and Abundance Ratio of Hydrocarbon Compounds at Different Temperatures (온도 변수에 대한 유류의 휘발특성 및 탄화수소 화합물의 존재비에 관한 연구)

  • Choi, Jung-Sik
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.27 no.7
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    • pp.1116-1123
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    • 2021
  • Oil spilled in seawater undergoes physical and chemical changes as well as biological degradation through various weathering processes, such as evaporation, diffusion, dispersion, emulsification, dissolution, oxidation, and sedimentation. Evaporation is one of the most immediate and prompt weathering processes, and it has the greatest influence on majority of pollutants. In this study, the evaporation characteristics of different oil samples were studied; the volatilization characteristics of gasoline, kerosene, and diesel were compared at average seawater (25 ℃) and near-equator (35 ℃) temperatures. The oil samples were pre-treated and then collected at regular intervals. Gas chromatography-mass spectrometry analysis was performed, and the changes in the amount of the hydrocarbons were calculated.

Simultaneous Determination of 285 Chemicals in Water at ppt Levels by GC-Ion Trap Mass Spectrometry

  • Kadokami, Kiwao;Sato, Kenji;Koga, Minoru;Shinohara, Ryota
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.771-778
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    • 1995
  • The authors have developed an analytical method for determining trace amounts of 285 kinds of chemicals in natural waters by GC-ion trap MS. The results of overall recovery tests at $0.1{\mu}g/l$ showed that the mean recovery was 92.1% and the mean relative standard deviation was 10.8%. The mean of the method detection limits was $0.036{\mu}g/l$. From the results of analysis of real samples, it was confirmed that this method is useful to elucidate the concentration levels and the fate of chemicals in the aquatic environment.

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Determination of Acaricides in Honey by Solid-Phase Extraction and Gas Chromatography / Mass Spectrometry

  • Hong, Joo-Yeon;Jung, Ok-Sang;Ryoo, Jae-Jeong;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.61-66
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    • 2009
  • An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

Discrimination of American ginseng and Asian ginseng using electronic nose and gas chromatography-mass spectrometry coupled with chemometrics

  • Cui, Shaoqing;Wu, Jianfeng;Wang, Jun;Wang, Xinlei
    • Journal of Ginseng Research
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    • v.41 no.1
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    • pp.85-95
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    • 2017
  • Background: American ginseng (Panax quinquefolius L.) and Asian ginseng (Panax ginseng Meyer) products, such as slices, have a similar appearance, but they have significantly different prices, leading to widespread adulteration in the commercial market. Their aroma characteristics are attracting increasing attention and are supposed to be effective and nondestructive markers to determine adulteration. Methods: The aroma characteristics of American and Asian ginseng were investigated using gas chromatography-mass spectrometry(GC-MS) and an electronic nose (E-nose). Their volatile organic compounds were separated, classified, compared, and analyzed with different pattern recognition. Results: The E-nose showed a good performance in grouping with a principle component analysis explaining 94.45% of variance. A total of 69 aroma components were identified by GC-MS, with 35.6% common components and 64.6% special ingredients between the two ginsengs. It was observed that the components and the number of terpenes and alcohols were markedly different, indicating possible reasons for their difference. The results of pattern recognition confirmed that the E-nose processing result is similar to that of GC-MS. The interrelation between aroma constituents and sensors indicated that special sensors were highly related to some terpenes and alcohols. Accordingly, the contents of selected constituents were accurately predicted by corresponding sensors with most $R^2$ reaching 90%. Conclusion: Combined with advanced chemometrics, the E-nose is capable of discriminating between American and Asian ginseng in both qualitative and quantitative angles, presenting an accurate, rapid, and nondestructive reference approach.

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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Analysis of Volatile Flavor Compounds in Milk Using Electronic Nose System (전자코 시스템을 이용한 우유의 품질에 따른 휘발성 향기성분 분석)

  • Kang, Nae Kyung;Jun, Tae-Sun;Yang, Yoon Seok;Kim, Yong Shin
    • Journal of Sensor Science and Technology
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    • v.23 no.5
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    • pp.320-325
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    • 2014
  • Volatile flavor compounds from milk were analyzed and identified by using the analysis methods of headspace solid phase microextraction gas chromatography/mass spectrometry (HSPME-GC/MS) and electronic nose (E-Nose) system. About 30 volatile compounds were identified by HSPME-GC/MS for the fresh and off-flavor milk samples. Also, the correlation between rancidity and ageing days of milk was obtained by the aid of principal component analysis algorithm. It shows that the E-Nose system can identify the various types of milk flavor. These results imply that the analysis method based on the E-nose system can apply to the quality control of milk flavor and the rancidity.

Development of Fingerprints for Quality Control of Acorus species by Gas Chromatography/Mass Spectrometry

  • Yu, Se-Mi;Kim, Eun-Kyung;Lee, Je-Hyun;Lee, Kang-Ro;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.32 no.5
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    • pp.1547-1553
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    • 2011
  • An effective analytical method of gas chromatography/mass spectrometry (GC/MS) was developed for the rapid determination of essential oils in the crude extract of Acorus species (Acorus gramineus, Acorus tatarinowii, and Acorus calamus). Major phenypropanoids (${\beta}$,${\alpha}$-asarone isomers, euasarone, and methyleugenol) and ${\beta}$-caryophyllene in Acorus species were used as marker compounds and determined for the quality control of herbal medicines. To extract marker compounds, various extraction techniques such as solvent immersion, mechanical shaking, and sonication were compared, and the greatest efficiency was observed with sonication extraction using petroleum ether. The dynamic range of the GC/MS method depended on the specific analyte; acceptable quantification was obtained between 10 and 2000 ${\mu}g/mL$ for ${\beta}$-asarone, 10 and 500 ${\mu}g/mL$ for ${\alpha}$-asarone, 10 and 200 ${\mu}g/mL$ for methyleugenol, and between 5 and 100 ${\mu}g/mL$ for ${\beta}$-caryophyllene. The method was deemed satisfactory by inter- and intra-day validation and exhibited both high accuracy and precision, with a relative standard deviation < 10%. Overall limits of detection were approximately 0.34-0.83 ${\mu}g/mL$, with a standard deviation (${\sigma}$)-to-calibration slope (s) ratio (${\sigma}$/s) of 3. The limit of quantitation in our experiments was approximately 1.13-3.20 ${\mu}g/mL$ at a ${\sigma}$/s of 10. On the basement of method validation, 20 samples of Acorus species collected from markets in Korea were monitored for the quality control. In addition, principal component analysis (PCA) and hierarchical cluster analysis (HCA) were performed on the analytical data of 20 different Acorus species samples in order to classify samples that were collected from different regions.