• Title/Summary/Keyword: GC/MS spectrometry

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Determination of Mequitazine in Human Plasma by Gas-Chro-matography/Mass Spectrometry with Ion-Trap Detector and Its Pharmacokinetics after Oral Administration to Volunteers

  • Kwon Oh-Seung;Kim Hye-Jung;Pyo Heesoo;Chung Suk-Jae;Chung Youn Bok
    • Archives of Pharmacal Research
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    • v.28 no.10
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    • pp.1190-1195
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    • 2005
  • The objective of this study was to develop an assay for mequitazine (MQZ) for the study of the bioavailability of the drug in human subjects. Using one mL of human plasma, the pH of the sample was adjusted and MQZ in the aqueous phase extracted with hexane; the organic layer was then evaporated to dryness, reconstituted and an aliquot introduced to a gas chromatograph/mass spectrometer (GC/MS) system with ion-trap detector. Inter- and intra-day precision of the assay were less than 15.1 and $17.7{\%}$, respectively; Inter- and intra-day accuracy were less than 8.91 and $18.6{\%}$, respectively. The limit of quantification for the current assay was set at 1 ng/mL. To determine whether the current assay is applicable in a pharmacokinetic study for MQZ in human, oral formulation containing 10 mg MQZ was administered to healthy male subjects and blood samples collected. The current assay was able to quantify MQZ levels in most of the samples. The maximum concentration ($C_{max}$ was 8.5 ng/mL, which was obtained at 10.1 h, with mean half-life of approximately 45.5 h. Under the current sampling protocol, the ratio of $AUC_{t{\rightarrow}last}$ to $AUC_{t{\rightarrow}{\infty}}$ was $934{\%}$, indicating that the blood collection time of 216 h is reasonable for MQZ. Therefore, these observations indicate that an assay for MQZ in human plasma is developed by using GC/MS with ion-trap detector and validated for the study of pharmacokinetics of single oral dose of 10 mg MQZ, and that the current study design for the bioavailability study is adequate for the drug.

Characteristics of Bio-oil by Pyrolysis with Pig Feces (돈분을 이용한 열분해공정 바이오오일의 특성)

  • Kun, Zhu;Choi, Hong L.
    • Journal of the Korea Organic Resources Recycling Association
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    • v.16 no.4
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    • pp.57-63
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    • 2008
  • The characteristics of the bio-oil produced by the pyrolysis process with pig feces was investigated in this paper. The continuous auger-type reactor produced bio-oil was maintained at the temperature range of 400 to $600^{\circ}C$, which was higher than a typical that in a conventional pyrolysis system. The pig feces was used as the feedstock. The bio-oil and its compositions were characterized by water analysis, heating values, elemental analysis, bio-oil compounds, by Gas Chromatography/Mass Spectrometry (GC/MS), and functional group by $^1H$ NMR spectroscopy. It was found that the maximum bio-oil yields of 21% w.t. was achieved at $550^{\circ}C$. This result suggested that this auger reactor might be a potential technology for livestock waste treatment to produce bio-oil because it is able to be improved to reach higher efficiency of bio-oil production in further study. The pyrolysis system reported herein had low heat transfer into the feedstock in the auger reactor so that it needs improve the heat conduction rate of the system in further study.

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Quantitative Analysis of ${\gamma}-oryzanol$ in Rice Bran (미강의 약리성분 감마-오리자놀의 정량)

  • Kwak, Tae-Soon;Park, Hee-Juhn
    • Korean Journal of Medicinal Crop Science
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    • v.5 no.2
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    • pp.113-118
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    • 1997
  • Phytochemical analysis on rice bran and its pitch was performed by the tool of TLC, UV- and IR-spetroscopy, so that it was found that they contained ${\gamma}-oryzanol$ and free sterol. GC-MS analysis of free sterol revealed that it was composed of ${\beta}-sitosterol$, campesterol and stigmasterol. Successive phytochemical analysis of ${\gamma}-oryzanol$ revealed that it was composed of ferulic acid ester of triterpene and sterol, respectively. Triterpene moieties of ${\gamma}-oryzanol$ were identified as follows: cycloartanol, cycloartenol, 24-methylenecycloartanol and unknown triterpene; And sterol moieties were found to be identical with free sterols. In addition, characteristic absorption band in UV spectrum (220-340 nm) was exclusively due to ${\gamma}-oryzanol$. Thus, it was suggested that rice brans of nearly all species of Oryza sativa can be quantitatively analyzed by UV absorption spectrometry, even when water soluble pigments was contained in the rice bran.

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Discriminating Eggs from Two Local Breeds Based on Fatty Acid Profile and Flavor Characteristics Combined with Classification Algorithms

  • Dong, Xiao-Guang;Gao, Li-Bing;Zhang, Hai-Jun;Wang, Jing;Qiu, Kai;Qi, Guang-Hai;Wu, Shu-Geng
    • Food Science of Animal Resources
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    • v.41 no.6
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    • pp.936-949
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    • 2021
  • This study discriminated fatty acid profile and flavor characteristics of Beijing You Chicken (BYC) as a precious local breed and Dwarf Beijing You Chicken (DBYC) eggs. Fatty acid profile and flavor characteristics were analyzed to identify differences between BYC and DBYC eggs. Four classification algorithms were used to build classification models. Arachidic acid, oleic acid (OA), eicosatrienoic acid, docosapentaenoic acid (DPA), hexadecenoic acid, monounsaturated fatty acids (MUFA), polyunsaturated fatty acids (PUFA), unsaturated fatty acids (UFA) and 35 volatile compounds had significant differences in fatty acids and volatile compounds by gas chromatography-mass spectrometry (GC-MS) (p<0.05). For fatty acid data, k-nearest neighbor (KNN) and support vector machine (SVM) got 91.7% classification accuracy. SPME-GC-MS data failed in classification models. For electronic nose data, classification accuracy of KNN, linear discriminant analysis (LDA), SVM and decision tree was all 100%. The overall results indicated that BYC and DBYC eggs could be discriminated based on electronic nose with suitable classification algorithms. This research compared the differentiation of the fatty acid profile and volatile compounds of various egg yolks. The results could be applied to evaluate egg nutrition and distinguish avian eggs.

Amphetamine-type Stimulants in Drug Testing

  • Chung, Heesun;Choe, Sanggil
    • Mass Spectrometry Letters
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    • v.10 no.1
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    • pp.1-10
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    • 2019
  • Amphetamine-type stimulants (ATS) are a group of ${\beta}$-phenethylamine derivatives that produce central nervous system stimulants effects. The representative ATS are methamphetamine and 3, 4-methylenedioxymethamphetamine (MDMA), and abuse of ATS has become a global problem. Methamphetamine is abused in North America and Asia, while amphetamine and 3, 4-methyle nedioxym ethamphetamine (Ecstasy) are abused in Europe and Australia. Methamphetamine is also the most abused drug in Korea. In addition to the conventional ATS, new psychoactive substances (NPS) including phenethylamines and synthetic cathinones, which have similar effects and chemical structure to ATS, continue to spread to the global market since 2009, and more than 739 NPS have been identified. For the analysis of ATS, two tests that have different theoretical principles have to be conducted, and screening tests by immunoassay and confirmatory tests using GC/MS or LC/MS are the global standard methods. As most ATS have a chiral center, enantiomer separation is an important point in forensic analysis, and it can be conducted using chiral derivatization reagents or chiral columns. In order to respond to the growing drug crime, it is necessary to develop a fast and efficient analytical method.

Volatile Flavor Components of Youngia denticulata and Amaranthus lividus (이고들빼기와 개비름의 휘발성 풍미성분)

  • Lee, Mie-Soon;Kim, Mi-Kyung
    • Korean Journal of Food Science and Technology
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    • v.21 no.4
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    • pp.511-514
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    • 1989
  • Volatile components of Youngia denticulata and Amaranthus lividus, Korean wild vegetables, were collected by Steam Distillation-Extraction (SDE) method Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Thirty one components, Including 10 alcohols, 2 esters, 6 aldehydes, 5 ketones, 3 hydrocarbons, 2 acids and 3 miscellaneous ones were confirmed in Youngia denticulata. Fifty eight components, including 12 alcohols, 4 esters, 5 aldehydes, 9 ketones, 3 acids, 2 phenols and 6 miscellaneous ones were confirmed in Amaranthus lividus.

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Thermal Stability Improvement of Liquid Fuel by Using Some Additives (첨가제를 이용한 액체연료의 열안정성 향상)

  • Park, Sun-Hee;Kim, Joong-Yeon;Chun, Byung-Hee;Han, Jeong-Sik;Jeong, Byung-Hun;Kim, Sung-Hyun
    • Journal of the Korean Society of Propulsion Engineers
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    • v.15 no.5
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    • pp.48-53
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    • 2011
  • We investigated thermal stability improvement of exo-tetrahydrodicyclopentadiene (exo-THDCP) with thermal stabilizers (additives). The reaction products were sample during the reactions. The compositions of products were determined by gas chromatography-mass spectrometry (GC-MS) to measure thermal decomposition products of exo-THDCP and to specify mechanism for thermal stabilizers. Hydrogen donors (thermal stabilizers) such as 1,2,3,4-tetrahydroquinoline (THQ), benzyl alcohol (BnOH) increased thermal stability of exo-THDCP. These materials donated hydrogen to radical of exo-THDCP produced after initiation of exo-THDCP. We found that stabilization of exo-THDCP radicals decreased activity of primary products of exo-THDCP and lowered formation of secondary products (above-$C_{11}$ products).

Measurement of 1,4-dioxane in surface water by headspace GC-MS (GC-MS에 의한 지표수에서 1,4-Dioxane의 측정)

  • Hong, Seon-Haw;Lee, Jun-Bae;Lee, Soo-Hyung;Lim, Hyun-Hee;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.27 no.1
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    • pp.22-26
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    • 2014
  • 1,4-Dioxane was classified as a Group 2B carcinogen by the International Agency for Research on Cancer. The compound was measured in surface water with a headspace gas chromatographic mass spectrometric detection. A 5 mL water sample was placed in a 10 mL headspace vial and saturated with NaCl, and the solution was spiked with 1,4-dioxane-d8 as an internal standard and sealed with a cap. Water samples were collected from twenty-two basins of Gum-River on June and September 2012, respectively. As a result, 1,4-dioxane was detected in the concentration range of $0.49-43.0{\mu}g/L$ (mean $2.0{\mu}g/L$) in the frequency of about 30% in surface water samples.

A Study on Remaining Formaldehyde Concentration in the Synthesis of Self-Healing Microcapsules (자기치유성 마이크로캡슐 합성 공정에서의 포름알데히드 잔류량 연구)

  • Kim, Dong-Min;Lee, Jun-Seo;Ryu, Byung-Cheol;Chung, Chan-Moon
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.8 no.1
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    • pp.129-133
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    • 2020
  • The concentration of remaining formaldehyde contained in waste liquid emitted from the process of urea-formaldehyde microcapsule synthesis was analyzed by gas chromatography-mass spectrometry (GC-MS). Three factors that can affect on the reaction of formaldehyde were selected including pH, ammonium chloride input and temperature. The effect of these factors on the concentration of remaining formaldehyde was studied. When ammonium chloride input was 0.025g, microcapsules could not be obtained or core substance leaked out because of weak shell, and therefore this reaction condition would be inadequate. It was confirmed that the concentration of remaining formaldehyde could be minimized when the microencapsulation was conducted at 70℃ and pH 2.5 by using a ammonium chloride input of 0.050g. This study can make contribution to UF microencapsulation in safer working environment.

Extraction Characteristics of Dried Asian Lacquer by Solvents Before and After UV Degradation (자외선 열화 전후 건조 옻의 용매별 용출 특성)

  • Park, Jongseo;Schilling, Michael R.;Khanjian, Herant;Heginbotham, Arlen
    • Journal of Conservation Science
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    • v.36 no.2
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    • pp.103-111
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    • 2020
  • To compare the cleaning effect of solvents such as water and ethanol used to clean lacquer relics, the components extracted with various solvents were analyzed. A freshly dried lacquer sample and a lacquer sample exposed to ultraviolet radiation for 24 days were treated with water, ethanol, acetone, and hexane, and the dissolved material was detected by pyrolysis-gas chromatography-mass spectrometry. The amount extracted was significantly higher in acetone and ethanol than in hexane, a nonpolar solvent. Water, a highly polar solvent, was relatively efficient for extracting low-molecular-weight materials. After experiencing 24 days of ultraviolet radiation, the lacquer exhibited a significant increase of extracted materials compared with the nonexposed one. This may be due to the degradation of the urushiol chain in the form of polymers, resulting in the formation of low-molecular-weight polar substances, including dicarboxylic acids. In addition to the deterioration status of lacquer relics, such solvent extraction properties will be a crucial consideration in selecting the appropriate cleaning solvent.