• Title/Summary/Keyword: Reaction monitoring

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Contamination of Sediments and Histological Alterations in Barfin Plaice Pleuronectes pinnifasciatus from Amursky Bay(Peter the Great Bay, East Sea/Sea of Japan)

  • Vaschenko Marina A.;Syasina Iraida G.;Durkina Valentina B.;Zhadan Petr M.
    • Ocean and Polar Research
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    • v.25 no.1
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    • pp.31-40
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    • 2003
  • In August-September 2001, 15 samples of bottom sediments were collected in the inner, middle and open parts of Amursky Bay near Vladivostok, Russia, and barfin plaice Pleuronectes pinnifasciatus was sampled from the inner and the middle locations of the bay. In the sediments from all three sites elevated concentrations of several heavy metals, i.e. Zn ($102-115{\mu}/g$ dry weight), Ni $(70-73{\mu}g/g)$ and Cu $(27-35{\mu}g/g)$ were discovered. The contents of oil hydrocarbons were very close to or slightly higher than the maximal normal environmental background level, $100{\mu}g/g$ dry weight. The sediments contained negligible amounts of hexachlorocyclohexane, while DDT concentrations were quite high (1.7-16.3ng/g dry weight). Generally, there were no substantial differences in the pollution levels of the locations studied and our results resembled those reported for Amursky Bay in the 1990s. Surprisingly, in 2001 'fiesh' DDT comprised 70-85% of the total DDT content in sediment from all the locations studied. In fish liver total DDTs concentrations were 212.8 and 122.54 ng/g wet weight for the inner and the middle locations, respectively, and 'fresh' DDT comprised 35 and 64% of DDTs, respectively. These results provide evidence of recent input of DDT from an unknown source into the ecosystem of Amursky Bay. Histopathological changes revealed in the plaice liver (vacuolization of hepatocytes, coagulative necrosis of hepatocytes, inflammatory reaction, and necrosis of epithelial cells of bile ducts) are probably connected with an intensive metabolism of DDT in the fish organism. No histological and histomorphometric differences were found in the state of the interrenal tissue. Similar condition of the liver and the interrenal tissue in barfin plaice sampled from the inner and the middle locations of Amursky Bay may be explained by the absence of great differences in the pollution levels of these sites.

Determination of Tiapride in Human Plasma Using Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry

  • Moon, Ya;Paek, In-Bok;Kim, Hui-Hyun;Ji, Hye-Young;Lee, Hye-Won;Park, Hyoung-Geun;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • v.27 no.9
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    • pp.901-905
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    • 2004
  • A rapid, sensitive and selective hydrophilic interaction liquid chromatography-tandem mass spectrometric(HILIC-MS/MS) method for the determination of tiapride in human plasma was developed. Tiapride and internal standard, metoclopramide were extracted from human plasma with dichloromethane at basic pH and analyzed on an Atlantis HILIC silica column with the mobile phase of acetonitrile-ammonium formate (190 mM, pH 3.0) (94:6, v/v). The ana-Iytes were detected using an electrospray ionization tandem mass spectrometry in the multi-ple-reaction-monitoring mode. The standard curve was linear (r=0.999) over the concentration range of 1.00-200 ng/mL. The coefficient of variation and relative error for intra- and inter-assay at three QC levels were 6.4∼8.8% and -2.0∼3.6%, respectively. The recoveries of tiapride ranged from 96.3 to 97.4%, with that of metoclopramide (internal standard) being 94.2%. The lower limit of quantification for tiapride was 1.00 ng/mL using 1 00 $\mu$L of plasma sample.

A Study on the Water Quality Relationship between Continuous Dam Discharge and Downstream in North Han River (북한강에 연속된 댐 구간 방류수와 하류 하천간 수질 관계 분석 연구)

  • Kim, Ji Won;Lee, Hye Won;Lee, Yong Seok;Choi, Jung Hyun
    • Journal of Korean Society on Water Environment
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    • v.36 no.2
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    • pp.89-97
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    • 2020
  • North Han River is a very unique type of water system, where Hwacheon, Chuncheon, Soyanggang, Euiam and Cheongpyeong Dams are located consecutively. These dams are operated differently in the amount of discharge and release schedule according to their structure and purpose of use. They have different water quality characteristics depending on external pollutant inflow and internal mixing condition. Therefore, this study investigated the relationship between the upper dam and down stream river with respect to water quality indicators, such as water temperature, electrical conductivity, BOD, COD, TN and TP of the North Han River. The similarities and correlations representing the relationship were analyzed by Pearson's correlation r and t-test. The data was taken from the Ministry of Environment's water quality monitoring from 1999 to 2018. The results show that water temperature and electrical conductivity of the dam and river are similar and correlated. However, it turned out that there was no similarities and correlations in BOD, COD, TN and TP that are significantly affected by subaqueous reaction mechanism. The results of this study present the impact of the dam on the water quality of North Han River, which can be used as useful data for management of water quality.

Toxoplasmic meningoencephalitis in a stray cat in Korea

  • Kim, Ha-Young;Bae, You-Chan;Woo, Gye-Hyeong;Byun, Jae-Won;Jung, Byeong-Yeal;Park, Jung-Won;Chae, Hee-Sun;Choi, Jae-Yong;Nakayama, Hiroyuki;Hwang, Eui Kyung;Joo, Yi-Seok;Lee, O-Soo
    • Korean Journal of Veterinary Research
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    • v.49 no.4
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    • pp.291-295
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    • 2009
  • A dead stray cat was necropsied for zoonotic feline disease monitoring. Grossly, there were no specific lesions. Major microscopic lesions included lymphocytic meningoencephalitis, malacia, and tissue cysts in the cerebral and cerebellar cortex. The size and shape of tissue cysts were identical to those of Apicomplexa including Toxoplasma (T.) gondii. Bradyzoites in the tissue cyst were strongly positive for T. gondii by immunohistochemistry. Electron microscopy revealed that bradyzoites within the tissue cyst were similar to the morphological features of T. gondii. Fresh tissue samples were examined by a polymerase chain reaction assay and resulted in a specific band of T. gondii only in the brain. Based on the results, this case was diagnosed as toxoplasmosis. This is the first case of toxoplasmic meningoencephalitis in a cat in Korea.

Quantitative Evaluation of Radix Astragali through the Simultaneous Determination of Bioactive Isoflavonoids and Saponins by HPLC/UV and LC-ESI-MS/MS

  • Kim, Jin-Hee;Park, So-Young;Lim, Hyun-Kyun;Park, Ah-Yeon;Kim, Ju-Sun;Kang, Sam-Sik;Youm, Jeong-Rok;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.28 no.7
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    • pp.1187-1194
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    • 2007
  • The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. These methods were fully validated with respect to the linearity, accuracy, precision, recovery and robustness. The HPLC/UV method was applied successfully to the quantification of three major isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry

  • Lee, Hyounyoung;Lim, Heungyoul;Yang, Juhong;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3629-3634
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    • 2013
  • In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.

Coupling of W-Doped SnO2 and TiO2 for Efficient Visible-Light Photocatalysis

  • Rawal, Sher Bahadur;Ojha, Devi Prashad;Choi, Young Sik;Lee, Wan In
    • Bulletin of the Korean Chemical Society
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    • v.35 no.3
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    • pp.913-918
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    • 2014
  • Five mol % tungsten-doped tin oxide ($W_{0.05}Sn_{0.95}O_2$, TTO5) was prepared by co-precipitation of $SnCl_4{\cdot}5H_2O$ and $WCl_4$, followed by calcination at $1000^{\circ}C$. The as-prepared TTO5 was in the pure cassiterite phase with a particle size of ~50 nm and optical bandgap of 2.51 eV. Herein it was applied for the formation of TTO5/$TiO_2$ heterojunctions by covering the TTO5 surface with $TiO_2$ by sol-gel method. Under visible-light irradiation (${\lambda}{\geq}420$ nm), TTO5/$TiO_2$ showed a significantly high photocatalytic activity in removing gaseous 2-propanol (IP) and evolving $CO_2$. It is deduced that its high visible-light activity is caused by inter-semiconductor holetransfer between the valence band (VB) of TTO5 and $TiO_2$, since the TTO5 nanoparticle (NP) exhibits the absorption edge at ~450 nm and its VB level is located more positive side than that of $TiO_2$. The evidence for the hole-transport mechanism between TTO5 and $TiO_2$ was also investigated by monitoring the holescavenging reaction with 1,4-terephthalic acid (TA).

Development of Isotope Dilution LC-MS/MS Method for Accurate Determination of Arsenobetaine in Oyster Certified Reference Material

  • Lee, Woo Young;Yim, Yong-Hyeon;Hwang, Euijin;Lim, Youngran;Kim, Tae Kyu;Lee, Kyoung-Seok
    • Bulletin of the Korean Chemical Society
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    • v.35 no.3
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    • pp.821-827
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    • 2014
  • An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, ${(CH_3)_3}^+AsCH_2COO^-$) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using $^{13}C_2$-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as $6.60mg{\cdot}kg^{-1}{\pm}0.31mg{\cdot}kg^{-1}$ and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.

Propofol Target Controlled Infusion (TCI) Sedation for Dental Treatment in the Exaggerated Gag Reflex Patient (심한 구역반사를 가진 성인환자에서 프로포폴 목표농도 주입법으로 시행한 깊은 진정)

  • Shin, Soonyoung;Cha, Min-Joo;Seo, Kwang-Suk;Kim, Hyun-Jeong;Lee, Jung-Man;Chang, Juhea
    • Journal of The Korean Dental Society of Anesthesiology
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    • v.12 no.2
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    • pp.105-109
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    • 2012
  • The gag reflex is a physiological reaction, but, an exaggerated gag reflex can be a severe limitation not only to treat dental caries but also to do oral exam. Procedures such as surface anesthesia of the palate and pharyngeral area, sedation, or general anesthesia can be options as behavioral management. But, there are no golden rule for the sever gag reflex patients. We present a case report of propofol intravenous sedation using TCI pump for simple dental treatment. A 44-year-old man, who had past history of general anesthesia for dental treatment because of severe gag reflex, was scheduled intravenous sedation for simple dental treatment. After 8 hour fasting he entered the clinic for persons with disabilities. We explained about intravenous deep sedation and got informed consent. First, we kept intravenous catheter (22G) in the arm and started monitoring ECG, non-invasive blood pressure, pulse oximetry and end-tidal $CO_2$ through nasal cannula. We started propofol infusion with TCI pump at the target concentration of 3 mcg/ml. The patient became sedated, but he showed involuntary movement during dental treatment, so we increased the target concentration to 4 mcg/ml. We finished the dental treatment without complications during 30 min. And after 40 min recovery room stay he was discharged without any complications.

Quantitative and Rapid Analysis of Transglutaminase Activity Using Protein Arrays in Mammalian Cells

  • Kwon, Mi-Hye;Jung, Jae-Wan;Jung, Se-Hui;Park, Jin-Young;Kim, Young-Myeong;Ha, Kwon-Soo
    • Molecules and Cells
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    • v.27 no.3
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    • pp.337-343
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    • 2009
  • We developed a novel on-chip activity assay using protein arrays for quantitative and rapid analysis of transglutaminase activity in mammalian cells. Transglutaminases are a family of $Ca^{2+}$-dependent enzymes involved in cell regulation as well as human diseases such as neurodegenerative disorders, inflammatory diseases and tumor progression. We fabricated the protein arrays by immobilizing N,N'-dimethylcasein (a substrate) on the amine surface of the arrays. We initiated transamidating reaction on the protein arrays and determined the transglutaminase activity by analyzing the fluorescence intensity of biotinylated casein. The on-chip transglutaminase activity assay was proved to be much more sensitive than the $[^3H]putrescine$-incorporation assay. We successfully applied the on-chip assay to a rapid and quantitative analysis of the transglutaminase activity in all-trans retinoic acid-treated NIH 3T3 and SH-SY5Y cells. In addition, the on-chip transglutaminase activity assay was sufficiently sensitive to determine the transglutaminase activity in eleven mammalian cell lines. Thus, this novel on-chip transglutaminase activity assay was confirmed to be a sensitive and high-throughput approach to investigating the roles of transglutaminase in cellular signaling, and, moreover, it is likely to have a strong potential for monitoring human diseases.