• Title/Summary/Keyword: gas chromatograph

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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.

THE LEVEL OF RESIDUAL MONOMER IN INJECTION MOLDED DENTURE BASE MATERIALS

  • Lee Hyeok-Jae;Kim Chang-Whe;Kim Yung-Soo
    • The Journal of Korean Academy of Prosthodontics
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    • v.41 no.3
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    • pp.360-368
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    • 2003
  • Statement of Problem: The residual monomer of denture base materials causes hypersensitivity on oral mucosa and intereferes with the mechanical properties of the cured resin. The amount of residual monomer is influenced by materials, curing cycle, processing method, and etc. Purpose: The aim of this study was to investigate the residual methyl methacrylate(MMA) content of injection molded denture base polymer, and to compare this with the self-cured resin and the conventional compression molded heat-cured resin. Materials and Methods: Disc shaped test specimens (50mm in diameter and 3mm thick) were prepared in a conventional flasking technique with gypsum molding. One autopolymerized denture base resins (Vertex Sc. Dentimex. Netherlands) and two heat-cured denture base resins (Vertex RS. Dentimex. Netherlands, Ivocap. Ivoclar Vivadent, USA) were used. The three types of specimens were processed according to the manufacturer's instruction. After polymerization, all specimens were stored in the dark at room temperature for 7 days. There were 10 specimens in each of the test groups. 3-mm twist drills were used to obtain the resin samples and 650mg of the drilled sample were collected for each estimation. Gas chromatography (Agillent 6890 Plus Gas Chromatograph, Agillent Co, USA) was used to determine the residual MMA content of 10 test specimens of each three types of polymer. Results: The residual monomer content of injection molded denture base resins was $1.057{\pm}0.141%$. The residual monomer content of injection molded denture base resins was higher than that of compression molded heat cured resin ($0.867{\pm}0.169%$). However, there was no statistical significant difference between two groups (p>0.01). The level of residual monomer in self cured resin($3.675{\pm}0.791$) was higher than those of injection molded and compression molded heat cured resins (p<0.01). Conclusion: With respect to ISO specification pass / fail test (2.2% mass fraction) of residual monomer, injection molding technique($1.057{\pm}0.141%$) is a clinically useful and safe technique in terms of residual monomer.

Feasibility study of membrane interface for gas chromatograph-mass spectrometry (기체크로마토그래프-질량분석기의 실리콘 분리막 인터페이스의 유용성 연구)

  • Kang, Gil Seon;Lee, Dong Soo;Lee, Hwa Sim;Park, Chang Joon
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.495-501
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    • 2008
  • Agilent 5973 GC-MS instrument was modified so that the capillary direct interface was removed and that a silicone membrane was installed between GC and MS. Feasibility study of the membrane interface GC-MS has been carried out. Vacuum of the mass spectrometer was not affected by the carrier gas flow rate up to $4.7m{\ell}/min$. As the carrier flow rate was increased, peak tailing was reduced and chromatogram peaks appeared earlier. Chromatogram peaks showed better separation and higher sensitivity as the membrane thickness was reduced from $127{\mu}m$ to $75{\mu}m$, and also as the interface temperature was increased. However, the membrane interface GC-MS had drawbacks such as background ions at 73 and 147 m/z and poor peak separation due to peak tailing.

Evaluation of the Giggenbach Bottle Method with Artificial Fumarolic Gases (인공 분기공 가스를 이용한 Giggenbach bottle 법의 평가)

  • Lee, Sangchul;Kang, Jungchun;Yun, Sung Hyo;Jeong, Hoon Young
    • Journal of the Korean earth science society
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    • v.34 no.7
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    • pp.681-692
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    • 2013
  • We aimed to evaluate the effectiveness of the Giggenbach bottle method and develop the related pretreatment and analytical methods using artificial fumarolic gases. The artificial fumarolic gases were generated by mixing $CO_2$, CO, $H_2S$, $SO_2$, $H_2$, and $CH_4$ gas streams with a $N_2$ stream sparged through an acidic medium containing HCl and HF, with their compositions varied by adjusting the gas flow rates. The resultant fumarolic gases were collected into an evacuated bottle partially filled with a NaOH absorption solution. While non-condensible gases such as CO, $H_2S$, and $CH_4$ accumulated in the headspace of the bottle, acidic components including $CO_2$, $SO_2$, HCl, and HF that were dissolved into the alkaline solution. Like other acidic components, $H_2S$ also dissolved into the solution, but it reacted with dissolved $Cd^{2+}$ to precipitate as CdS when $Cd(CH_3COO)_2$ was added. The non-condensible gases were analyzed on a gas chromatography. Then, CdS precipitates were separated from the alkaline solution by filtration, and they were pretreated with $H_2O_2$ to oxidize CdS-bound sulfide into sulfate. In addition, a portion of the solution was also pretreated with $H_2O_2$ to oxidize sulfite to sulfate. Following the pretreatment, the resultant samples were analyzed for $SO_4^{2-}$, $Cl^-$ and $F^-$ on an ion chromatography. In the meanwhile, dissolved $CO_2$ was analyzed on a total organic carbon-inorganic carbon analyzer without such pretreatment. According to our experimental results, the measured concentrations of the fumarolic gases were shown to be proportional to the gas flow rates, indicating that the Giggenbach bottle method is adequate for monitoring volcanic gas. The pretreatment and analytical methods employed in this study may also enhance the accuracy and reproducibility of the Giggenbach bottle method.

In vitro evaluation of nano zinc oxide (nZnO) on mitigation of gaseous emissions

  • Sarker, Niloy Chandra;Keomanivong, Faithe;Borhan, Md.;Rahman, Shafiqur;Swanson, Kendall
    • Journal of Animal Science and Technology
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    • v.60 no.11
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    • pp.27.1-27.8
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    • 2018
  • Background: Enteric methane ($CH_4$) accounts for about 70% of total $CH_4$ emissions from the ruminant animals. Researchers are exploring ways to mitigate enteric $CH_4$ emissions from ruminants. Recently, nano zinc oxide (nZnO) has shown potential in reducing $CH_4$ and hydrogen sulfide ($H_2S$) production from the liquid manure under anaerobic storage conditions. Four different levels of nZnO and two types of feed were mixed with rumen fluid to investigate the efficacy of nZnO in mitigating gaseous production. Methods: All experiments with four replicates were conducted in batches in 250 mL glass bottles paired with the ANKOM$^{RF}$ wireless gas production monitoring system. Gas production was monitored continuously for 72 h at a constant temperature of $39{\pm}1^{\circ}C$ in a water bath. Headspace gas samples were collected using gas-tight syringes from the Tedlar bags connected to the glass bottles and analyzed for greenhouse gases ($CH_4$ and carbon dioxide-$CO_2$) and $H_2S$ concentrations. $CH_4$ and $CO_2$ gas concentrations were analyzed using an SRI-8610 Gas Chromatograph and $H_2S$ concentrations were measured using a Jerome 631X meter. At the same time, substrate (i.e. mixed rumen fluid+ NP treatment+ feed composite) samples were collected from the glass bottles at the beginning and at the end of an experiment for bacterial counts, and volatile fatty acids (VFAs) analysis. Results: Compared to the control treatment the $H_2S$ and GHGs concentration reduction after 72 h of the tested nZnO levels varied between 4.89 to 53.65%. Additionally, 0.47 to 22.21% microbial population reduction was observed from the applied nZnO treatments. Application of nZnO at a rate of $1000{\mu}g\;g^{-1}$ have exhibited the highest amount of concentration reductions for all three gases and microbial population. Conclusion: Results suggest that both 500 and $1000{\mu}g\;g^{-1}$ nZnO application levels have the potential to reduce GHG and $H_2S$ concentrations.

Headspace Analysis for Residual Hexane in Vegetable Oil

  • Oh, Chang-Hwan;Kwon, Yong-Kwan;Jang, Young-Mi;Lee, Dal-Su;Park, Jong-Sei
    • Food Science and Biotechnology
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    • v.14 no.4
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    • pp.456-460
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    • 2005
  • To enforce the maximum residue limit for residual hexane (0.005 g/kg) in commercially available Korean vegetable oil, convenient and accurate quantification methods were investigated. Using dual surrogate standards, pentane and heptane were dissolved in ethanol, and then added to hexane-tree sunflower oil for setting up the calibration curve. Gas Chromatograph-Flame Ionization Detector with a porous layer open tubular column, indicated good chromatographic separation of hexane from other inhibiting matrix components. The lowest calibration level was $0.5\;{\mu}g/g$, not exceeding a relative standard deviation of 10% (RSD%), and 1.0\;{\mu}g/g$ not exceeding a deviation of 22% RSD% using heptane as an internal standard for the Static headspace analysis by using a headspace auto-sampler and manual injection, respectively. The residual hexane was detected in nine of the samples among 87 vegetable oil samples purchased on the local market.

Evaluation of Chemical Analysis Method and Determination of Polycyclic Aromatic Hydrocarbons Content from Seafood and Dairy Products

  • Lee, So-Young;Lee, Jee-Yeon;Shin, Han-Seung
    • Toxicological Research
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    • v.31 no.3
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    • pp.265-271
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    • 2015
  • This study was carried out to investigate contents of 8 polycyclic aromatic hydrocarbons (PAHs) from frequently consumed seafood and dairy products and to evaluate their chemical analysis methods. Samples were collected from markets of 9 cities in Korea chosen as the population reference and evaluated. The methodology involved saponification, extraction with n-hexane, clean-up on Sep-Pak silica cartridges and gas chromatograph-mass spectrometry analysis. Validation proceeded on 2 matrices. Recoveries for 8 PAHs ranged from 86.87 to 103.57%. The limit of detection (LOD) 8 PAHs was $0.04{\sim}0.20{\mu}g/kg$, and limit of quantification (LOQ) of 8 PAHs was $0.12{\sim}0.60{\mu}g/kg$. The mean concentration of benzo[a]pyrene (BaP) was $0.34{\mu}g/kg$ from seafood and $0.34{\mu}g/kg$ from dairy products. The total PAHs concentration was $1.06{\mu}g/kg$ in seafood and $1.52{\mu}g/kg$ in dairy products.

Determination of Organic Pollutants in Dyeing Wastewater (염색폐수 중의 유기오염물질 분석)

  • Yook, Keun-Sung
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.332-342
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    • 1997
  • Fifteen volatile organic pollutants were spiked in blank water at the concentration of $20{\mu}g/L$ and analyzed with Purge and Trap and GC/MS. As a result, the overall mean recovery of 100% was obtained with a mean relative standard deviation of 3.6%. The method detection limits were in the range of $1.9{\sim}3.3{\mu}g/L$. In the wastewater analysis of Banwol dyeing comlex, 15 organic compounds were identified and three of these were quantified. Among the compounds identified, only trichloroethylene and tetrachloroethylene are regulated in wastewater by the Korea Ministry of Environment. But, the concentration of these two compounds were below the government allowance level.

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Measurements of Peroxyacetyl Nitrates at an Urban and a Rural Site in Korea (도시지역과 청정지역에서의 대기 중 PAN(PeroxyAcetyl Nitrate) 측정)

  • 김세웅;이강웅;김경렬
    • Journal of Korean Society for Atmospheric Environment
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    • v.17 no.2
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    • pp.157-167
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    • 2001
  • Although PAN has ong been considered to belong to one of the most characteristic photooxidants, its concentra-tions have rarely been measured in a systematic manner in Korea. The first in-situ Measurements of PAN were made in concert with simultaneous analysis of NO, NO$_2$, $O_3$ and UV-Visible radiation intensity from Seoul and dong-Hae during Spring and early Summer of 1999. The aim of our study was to evaluate the behavior of photo-chemical species in a highly polluted urban air and a relative clean one. PAN were determined using a semi-auto-mated gas chromatograph equipped with an electron captured detection system. Calibration of the PAN was done by synthesizing liquid standards using a strong acid nitration of the corresponding peracid. The PAN concentra-tions were found in the range of a few ppbv in the urban air ad persistently less than a ppbv in the clean rural airs. Diurnal variations of PAN and $O_3$ were also observed consistently during the experiment with maxima occurring during the late daylight hours. While the positive dependency of $O_3$ production and PAN concentrations were ob-served in most occasion, the dependency became deviated significantly under changes in air masses.

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The Effect of Roasting Temperature on the Formation of Volatile Compounds in Chinese-Style Pork Jerky

  • Chen, W.S.;Liu, D.C.;Chen, M.T.
    • Asian-Australasian Journal of Animal Sciences
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    • v.15 no.3
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    • pp.427-431
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    • 2002
  • The purpose of this work was to study the effect of roasting temperature on the production of volatile compounds in Chinese-style pork jerky. The pork jerky was roasted by far-infrared grill at $150^{\circ}C$ or $200^{\circ}C$ for 5 min. The analysis of volatile compounds using a Likens-Nickerson apparatus coupled to a gas chromatograph and a mass spectrometer enabled us to identify 21 volatile compounds. The results showed that the volatile compounds coming from pork jerky can be divided into two groups in accordance with their possible origins. The first group of volatile compounds derived from oxidation of lipid included hexanal, ethylbenzene, nonanal, benzaldehyde, 2,4-decadienal, 1-octen-3-ol, octadecanal, and 9-octadecenal. The second group of volatile compounds generated from degradation of natural spices included 1,8-cinene, 4-terpineol, ${\alpha}$-terpineol, e-anethole, methyl-eugenol, panisaldehyde, elemol, eugenol, methyl-isoeugenol and myristicin. Significant differences (p<0.05) were found between 2 different roasted temperatures at levels for all volatile compounds.