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Gamakamide C and D as Two New Analogues of Bitter-Tasting Cyclic Peptide with Hydantoin Structure from Oyster Crassostrea gigas

  • Jang, Jun Ho;Park, Taesung;Lee, Jong Soo
    • Fisheries and Aquatic Sciences
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    • v.18 no.2
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    • pp.131-135
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    • 2015
  • Two new bitter-tasting cyclic peptides comprising six amino acids, namely gamakamide C and D, were isolated from cultured oysters Crassostrea gigas. Dimethylaminoazobenzene sulfonyl-amino acid analysis detected Val and Leu in gamakamide C and Ile and Leu in gamakamide D. The molecular formula of gamakamide C was determined as $C_{43}H_{60}N_{7}O_8S$ by high-resolution fast atom bombardment mass spectroscopy (HR FAB-MS) ($[M+H]^+m/z822.4200{\Delta}-2.4mmu$), and that of gamakamide D was determined as $C_{43}H_{62}N_7O_8S$ by HR FAB-MS ($[M+H]^+m/z836.4379{\Delta}-2.0mmu$). Comparison of amino acid analyses and fragment ions by MS/MS among gamakamide C, D, and E (known), the structures of gamakamide C and D were confirmed $as-{\small{L}}-Val-{\small{L}}-Met(SO)-{\small{L}}-NMe-Phe-{\small{L}}-Leu-{\small{D}}-Lys-{\small{L}}-Phe-$ and $-{\small{L}}-Ile-{\small{L}}-Met(SO)-{\small{L}}-NMe-Phe-{\small{L}}-Leu-{\small{D}}-Lys-{\small{L}}-Phe-$, respectively.

A Protocol for High Frequency Plant Conversion from Somatic Embryos of Peanut (Arachis hypogaea L. cv. DRG-12)

  • Rani A. Raja;Padmaja G.
    • Journal of Plant Biotechnology
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    • v.7 no.3
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    • pp.187-193
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    • 2005
  • A protocol was developed for somatic embryogenesis with 100% induction rate from immature zygotic embryo axes of peanut (Arachis hypogaea L. cv. DRG-12) cultured on MS medium containing $18.09\;{\mu}M$ 2,4-D. The frequency of somatic embryogenesis (31.7%) as well as the number of somatic embryos induced per explant (6.6) decreased when the concentration of 2,4-D was increased to $72.4\;{\mu}M$. Morphologically abnormal somatic embryos were observed at a frequency of 43.3% on MS medium containing $72.4\;{\mu}M$ 2,4-D. Somatic embryos isolated from 30-day-old cultures of immature zygotic embryo axes exhibited precocious germination with varied responses when placed on MS basal medium with 3% sucrose. Maximum shoot induction (80.0%) was observed from somatic embryos isolated from 60-day-old cultures of immature zygotic embryo axes when placed as a clump rather than individually on MS medium supplemented with $26.63\;{\mu}M$ BA and $0.54\;{\mu}M$ NAA. Shoots developed from somatic embryos rooted with higher frequency (93.3%) on Blaydes' medium containing $5.4\;{\mu}M$ NAA.

Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Lithospermic Acid B in Rat Serum

  • Kim, Hui-Hyun;Ji, Hye-Young;Lee, Hye-Won;Kim, Youn-Chul;Sohn, Dong-Hwan;Lee , Hye-Suk
    • Archives of Pharmacal Research
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    • v.27 no.12
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    • pp.1202-1206
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    • 2004
  • A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/ MS) method for the determination of lithospermic acid B (LSB) in rat serum was developed. LSB and internal standard, 7-hydroxy-3-phenyl-chromen-4-one (HPC) were extracted from rat serum with methyl-tert-butyl ether at acidic pH and analyzed on a Luna $C_8$ column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 6.5) (50:50, v/v). The analytes were detected using a negative electrospray ionization tandem mass spectrometry in the multiple- reaction-monitoring mode. The standard curve was linear $(r^2 = 0.997)$ over the concentration range of 10.0-500 ng/mL. The coefficient of variation and relative error for intra- and interassay at three QC levels were 1.1~6.2% and -10.3~-2.7%, respectively. The recovery of LSB from serum sample ranged from 73.2 to 79.5%, with that of HPC (internal standard) being 75.1 %. The lower limit of quantification for LSB was 10 ng/mL using 50 ${\mu}L$ of serum sample.

Bridge Resistance Deviation-to-Period Converter for Resistive Biosensors (저항형 바이오 센서를 위한 브릿지 저항 편차-주기 변환기)

  • Chung, Won-Sup
    • The Journal of Korea Institute of Information, Electronics, and Communication Technology
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    • v.7 no.1
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    • pp.40-44
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    • 2014
  • A bridge resistance deviation-to-period (BRD-to-P) converter is presented for interfacing resistive biosensors. It consists of a linear operational transconductance amplifier (OTA) and a current-controlled oscillator (CCO) formed by a current-tunable Schmitt trigger and an integrator. The free running period of the converter is 1.824 ms when the bridge offset resistance is $1k{\Omega}$. The conversion sensitivity of the converter amounts to $3.814ms/{\Omega}$ over the resistance deviation range of $0-1.2{\Omega}$. The linearity error of the conversion characteristic is less than ${\pm}0.004%$.

Quantitative Determination of Amitriptyline and Its Metabolite in Rat Plasma by Liquid Chromatography-tandem Mass Spectrometry

  • Chae, Jung-Woo;Baek, In-Hwan;An, Jung-Hwa;Kim, Eun-Jung;Kwon, Kwang-Il
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2163-2167
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    • 2012
  • A rapid, specific, and reliable LC-MS/MS-based bioanalytical method was developed and validated in rat plasma for the simultaneous quantitation of amitriptyline and its metabolite nortriptyline. Chromatographic separation of these analytes was achieved on a Gemini C18 column ($50{\times}4.60mm$, $5{\mu}m$) using reversed-phase chromatography. The mobile phase was an isocratic solvent system consisting of 1% formic acid in water and methanol (10:90, v/v), at a flow rate of 0.2 mL/min. The analytical range was set as 0.1-500 ng/mL for amitriptyline and 0.08-500 ng/mL for nortriptyline using a $200{\mu}L$ plasma sample. The accuracy and precision of the assay were in accordance with FDA regulations for the validation of bioanalytical methods. The validated method was successfully applied to a pharmacokinetic study in six rats after oral administration of amitriptyline (15 mg/kg). This method allows laboratory scientists to rapidly determine amitriptyline and nortriptyline concentrations in plasma.

Identification of Antioxidative Constituents from Polygonum aviculare using LC-MS Coupled with DPPH Assay

  • Shin, Hyeji;Chung, Hayeon;Park, Byoungduck;Lee, Ki Yong
    • Natural Product Sciences
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    • v.22 no.1
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    • pp.64-69
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    • 2016
  • A method for simultaneously identifying antioxidative compounds was developed using time-based LC-MS coupled with DPPH assay regardless of the time consuming process. The methanolic extract of Polygonum aviculare (Polygonaceae) showed significant DPPH radical scavenging activity. Time-based DPPH assay for simultaneous identification of active compounds from the extracts of P. aviculare was used. Major peaks of ethyl acetate fraction of P. aviculare showed high DPPH radical scavenging activity. A simple phenolic compound (1) and six flavonoids (2-7) were isolated from the ethyl acetate fraction of P. aviculare by silica gel and sephadex LH-20 column chromatography. The structures of seven compounds were determined to be protocatechuic acid (1), catechin (2), myricitrin (3), epicatechin-3-O-gallate (4), avicularin (5), quercitrin (6), and juglanin (7) based on the analysis of the $^1H$-NMR, $^{13}C$-NMR and ESI-MS data. All compounds exhibited significant antioxidant activity on DPPH assay and active compounds were well correlated with predicted one.

Determination of antibiotics by SPE-LC-MS/MS in wastewater and risk assessment

  • Aydin, Senar;Aydin, Mehmet E.;Ulvi, Arzu;Kilic, Havva
    • Advances in environmental research
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    • v.7 no.3
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    • pp.201-212
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    • 2018
  • In this study, conditions of solid phase extraction (SPE) for determination of some antibiotics such as trimethoprim, oxytetracycline, erythromycin, clarithromycin, azythromycin, doxycycline, sulfamethazine, ciprofloxacin, chlortetracycline, sulfamethoxazole in wastewaters were optimized. After the optimum volume and pH of the sample were determined, the effect of the concentration of the compounds and matrix were investigated. The highest recovery rates for antibiotic compounds were determined between 82% and 105% in 200 mL sample volume and pH 2.5. Then, antibiotic compounds were investigated in influent and effluent samples taken from Konya Urban Wastewater Treatment Plant. The concentration of the antibiotics was detected range of 0.11-101 ng/L in influent waters and

A study of the metabolites for 7-keto-DHEA-acetate in human urine (뇨시료에 함유된 7-keto-DHEA-acetate의 대사체에 관한 연구 (I))

  • Kim, Yunje;Lee, Jinhee
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.337-346
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    • 2004
  • 7-keto-dehydroepiandrosterone-acetate (7-keto-DHEA-acetate) is an anabolic steroids, and we studied basically to the metabolites of it after human dosing. We tested the matrix effect from human urine to detect the 7-keto-DHEA-acetate. And LC/ESI/MS and GC/MSD was used to detect the metabolites in dosed urine. We found the some unknown compound from dosed urine (M1, M2, M3, M4 and M5), and from these results, we supposed that these compounds have the more than 3 hydroxyl and/or ketone group. Metabolite M1 was supposed that molecular weight is 302 and 3-,17-diketone and 7-hydroxyl compound (7-OH-androstendione). Metabolite M2 was supposed that the molecular weight was same to M1 and 7-,17-diketone and 3-hydroxyl compound (7-keto-DHEA).

Analysis of Synthetic Fragrances (SFs) in Water Using Stir Bar Sorptive Extraction (SBSE) and GC-MS/MS (교반막대 추출법과 GC-MS/MS를 이용한 수중의 합성 향물질류 분석)

  • Seo, Chang-Dong;Son, Hee-Jong;Yoom, Hoon-Sik;Choi, Jin-Taek;Ryu, Dong-Choon;Kwon, Ki-Won;Jang, Seung-Ho
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.6
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    • pp.387-395
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    • 2014
  • A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC-MS/MS) has been developed, allowing the simultaneous multi-analyte determination of 11 synthetic fragrances (SFs) in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 10.9%). The extraction efficiencies were above 83% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~4.1 ng/L and 6.6~12.9 ng/L, respectively. The developed method offers the ability to detect 11 SFs at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 11 SFs. The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.

Sensitive determination of paroxetine in canine plasma by liquid chromatography-tandem mass spectrometry (LC-MS/MS) (LC-MS/MS를 이용한 비글견 혈장 중 파록세틴의 고감도 분석)

  • Chang, Kyu Young;Kang, Seung Woo;Han, Sang Beom;Youm, Jeong-Rok;Lee, Kyung Ryul;Lee, Hee Joo
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.138-146
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    • 2007
  • A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.