• Bulletin of the Korean Chemical Society
• /
• v.34 no.12
• /
• pp.3681-3689
• /
• 2013

This study explored a direct SET-photochemical strategy to construct a new family of thioene conjugated-naphthalamide fluorophore based lariat-crown ethers which show strong binding properties towards heavy metal ions. Irradiations of designed nitrogen branched (trimethylsilyl)methylthio-terminated polyethylenoxy-tethered naphthalimides in acidic methanol solutions have led to highly efficient photocyclization reactions to generate naphthalamide based lariat type thiadiazacrown ethers directly in chemo- and regio-selective manners which undergo very facile secondary dehydration reactions during separation processes to produce their corresponding amidoenethio ether cyclic products tethered with electron donating diethyleneoxy- and diethyenethio-side arm chains. Fluorescence and metal cation binding properties of the lariat type enamidothio products were examined. The photocyclized amidoenethio products, thioene conjugated naphthalamide fluorophore containing lariat-thiadiazacrowns exhibited strong fluorescence emissions in region of 330-450 nm along with intramolecular exciplex emissions in region of 450-560 nm with their maxima at 508 nm. Divalent cation $Hg^{2+}$ and $Pb^{2+}$ showed strong binding to sulfur atom(s) in side arm chain and atoms in enethiadiazacrown ether rings which led to significant enhancement of fluorescence from its chromophore singlet excited state and concomitant quenching of exciplex emission. The dual fluorescence emission responses towards divalent cations might provide a new guide for design and development of fluorescence sensors for detecting those metals.

• Toxicological Research
• /
• v.27 no.2
• /
• pp.125-131
• /
• 2011

Through the present study, we produced a monoclonal antibody against aflatoxin B1 (AFB1) using AFB1-carboxymethoxylamine BSA conjugates. One clone showing high binding ability was selected and it was applied to develop a direct competitive ELISA system. The epitope densities of AFB1-CMO against BSA and KLH were about 1 : 6 and 1 : 545, respectively. The monoclonal antibody (mAb) from cloned hybridoma cell was the IgG1 subclass with ${\lambda}$-type light chains. The $IC_{50}s$ of the monoclonal antibody developed for AFB1, AFB2, AFG1 and AFG2 were 4.36, 7.22, 6.61 and 29.41 ng/ml, respectively, based on the AFB1-KLH coated ELISA system and 15.28, 26.62, 32.75 and 56.67 ng/ml, respectively, based on the mAb coated ELISA. Cross-relativities of mAb to AFB1 for AFB2, AFG1 and AFG2 were 60.47, 65.97 and 14.83% in the AFB1-KLH coated ELISA, and 59.41, 46.66 and 26.97% in the mAb coated ELISA, respectively. Quantitative calculations for AFB1 from the AFB1-Ab ELISA and AFB1-Ag ELISA ranged from 0.25 to 25 ng/ml ($R^2$ > 0.99) and from 1 to 100 ng/ml ($R^2$ > 0.99), respectively. The intra- and inter-assay precision CVs were < 10% in both ELISA assay, representing good reproducibility of developed assay. Recoveries ranged from 79.18 to 91.27%, CVs ranged from 3.21 to 7.97% after spiking AFB1 at concentrations ranging from 5 to 50 ng/ml and following by extraction with 70% methanol solution in the Ab-coated ELISA. In conclusion, we produced a group specific mAb against aflatoxins and developed two direct competitive ELISAs for the detection of AFB1 in feeds based on a monoclonal antibody developed.

• Mass Spectrometry Letters
• /
• v.5 no.4
• /
• pp.104-109
• /
• 2014

Nonmedical use of prescription stimulants such as methylphenidate (MPH) and amphetamine (AP) by normal persons has been increased to improve cognitive functions. Due to high potential for their abuse, reliable analytical methods were required to detect these prescription stimulants in biological samples. A direct injection liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and implemented for simultaneous determination of MPH, AP and their metabolites ritalinic acid (RA) and 4-hydroxyamphetamine (HAP) in human urine. Urine sample was centrifuged and the upper layer ($100{\mu}L$) was mixed with $800{\mu}L$ of distilled water and $100{\mu}L$ of internal standards ($0.2{\mu}g/mL$ in methanol). The mixture was then directly injected into the LC-MS/MS system. The mobile phase was composed of 0.2% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Capcell Pak MG-II C18 ($150mm{\times}2.0mm$ i.d., $5{\mu}m$, Shiseido) column and all analytes were eluted within 5 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve and the assay was linear from 20 to 1500 ng/mL (HAP), 40-3000 ng/mL (AP and RA) and 2-150 ng/mL (MPH). The intra- and inter-day precisions were within 16.4%. The intra- and inter-day accuracies ranged from -15.6% to 10.8%. The limits of detection for all the analytes were less than 4.7 ng/mL. The suitability of the method was examined by analyzing urine samples from drug abusers.

• Korean Membrane Journal
• /
• v.9 no.1
• /
• pp.52-56
• /
• 2007

A proton exchange membrane was prepared by ${\gamma}-irradiation-induced$ grafting of styrene into poly(tetrafluoro-ethylene-co-perfluoropropyl vinyl ether) (PFA) and subsequent sulfonation reaction. The degree of grafting (DOG) increased with an increase in the absorbed dose. The prepared membranes showed high ion exchange capacity reaching 3.0 meq/g, which exceeded the performance of commercially available perfluorosulfonic acid membranes such as Nafion. The proton conductivity of PFA-g-PSSA membrane increased with the DOG and reached 0.17 S/cm for the highest sample at room temperature. The DMFC performance of the prepared membranes with 50% DOG was comparable to that of Nafion membrane.

• 한국신재생에너지학회:학술대회논문집
• /
• 2010.06a
• /
• pp.137.2-137.2
• /
• 2010

본 연구는 스테인리스 스틸(STS)을 직접메탄올 연료전지(DMFC)용 바이폴라 플레이트에 적용하기 위한 것이다. 약산성의 연료전지 환경에서 부식저항성을 향상시키고자 오스테나이트계 STS 316L과 페라이트계 STS 430에 UBM(unbalanced magnetron) DC sputter로 CrN 코팅막을 제작하였다. CrN이 코팅된 스테인리스 스틸은 부식특성, 접촉 저항 및 접촉각 등을 측정하여 무 코팅의 스테인리스 스틸과 특성을 비교하였다. 그리고 이들 재료의 연료전지(DMFC) 적용 가능성을 알아보기 위하여 단위전지로 제작하여 연료전지 성능 등을 측정하고 평가하였다. 무 코팅 스테인리스 스틸(STS 316L, STS 430)과 CrN 코팅 스테인리스 스틸의 부식저항 특성은 동전위와 정전위 실험으로 조사하였다. 동전위 부식 실험은 -0.4~1.0 V로 0.001 M의 황산용액 또는 메탄올을 첨가하여 질소 또는 공기의 환경에서 실험을 실시하였으며, 정전위 부식 실험은 0.4 V 또는 0.6 V에서 진행하였다. 연료전지의 단전지 측정은 실제 DMFC의 운전조건에서 실시하였다. 부식실험과 단전지 실험 전/후 메탈 바이폴라 플레이트의 조직 변화는 SEM을 통해 관찰하였고, 부식산화물의 화학적 조성과 메탈 바이폴라의 표면은 EDS를 이용하여 측정하였다.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.3 no.1
• /
• pp.69-76
• /
• 1974

The method of amino acid sequence determination from the C-terminal amino acid is proposed and mass spectrometric identification of thiohydantoins described previously. In this paper was discussed the fragmentation of thiohydantoin-ring by deutero substitution and model tripeptide have been degraded through three stages each, with interpretable results. The conditions employed in this method are mild enough for biological materials. The main features of the method are the following. 1. Thiohydantoins were formed in a non-aqueous medium a mixture of acetic anhydride, acetic acid and ammonium thiocyanate. 2. Mass sepectra of thiohydantoins derived from 20 amino acids were obtained with a mass spectrometer, JEOL model JMS-06H. 3. Cleavage of peptidyl thiohydantoin was made with an acidic from of a cation-exchange resin. (Amberlite IR-120) 4. Separation of the cleaved thiohydantoin and the parent peptide less one amino acid moiety was made by chromatography on a Sephadex G-10 column. 5. The peptide fraction was concentrated by freezedrying. 6. Thiohydantoin derivative of carboxyl terminal amino acid residue was introduced with a direct inlet probe in methanol solution.

• 한국신재생에너지학회:학술대회논문집
• /
• 2009.06a
• /
• pp.365-368
• /
• 2009

메탄올 연료전지에서 기존의 탄소 지지체의 전기화학적인 특성과 유사한 새로운 지지체 물질을 개발하기위해서 $TiO_2$ 산화물을 선정하였고 이것의 전도성을 향상에 관한 연구를 하였다. 새로운 지지체인 Degussa $TiO_2$를 이용하여 고온에서 열처리하는 방법으로써 얻을 수 있었다. 이러한 지지체위에 백금 촉매를 담지하는 합성 실험은 간단한 방법인 sodium borohydride 방법으로써 수행하였고 구조적인 결과를 확인하기 위하여 XRD 분석으로써 확인하였다. 결과로부터 $TiO_2$에서 TiN으로 구조적인 변화를 알 수 있었고 상변화 과정이 높은 에너지와 소스로 인해 바뀐다는 것을 알 수 있었다. 이러한 지지체 촉매 전극의 전기적인 활성을 알아보기 위하여 CVs와 안전성을 확인하기 위하여 CA에서 분석하였다. 기존 탄소 지지체 촉매 전극과 황산과 메탄올 용액하에서 CVs와 CA를 비교하였을 때, 티타늄 질화물 지지체가 CVs에서 유사한 산화, 환원 활성을 나타내었고 CA에서 높은 전류에서 안정성을 보여주었다. 이러한 결과로부터 TiN 지지체는 탄소 지지체와 비교하였을 때 연료전지의 지지체로써의 가능성을 확인 할 수 있었다.

• New & Renewable Energy
• /
• v.3 no.1 s.9
• /
• pp.60-67
• /
• 2007

Catalyst coated membrane [CCM] type and catalyst coated substrate [CCS] type of membrane electrode assembly [MEA] were manufactured and evaluated their performance. Degradation test were conducted to find the difference of long term stability in two types of MEA and the factor for performance degradation problem occurred. Performance degradation test of single cell in two different types of MEA were carried out when current density was $200mA/cm^{2}$. The degradation test had proceeded for 230 hours and performance degradation was checked by I-V curve and impedance measurement at regular intervals. Also, MEA before/after operation and changes of catalyst layer were characterized by SEM, TEM, and XRD. Maximum power density of CCM type was higher than that of CCS type. Meanwhile, an increase of particle size of catalyst and an increase of impedance resistance after long term operation were observed. In the case of using CCM type MEA, the performance was deteriorated 38% of initial performance. In the case of using CCS type MEA, the performance was deteriorated 43% of initial performance. In consideration of difference of initial performance, performance of CCM type is higher than that of CCS type but both types had similar problems during degradation test.

• 한국신재생에너지학회:학술대회논문집
• /
• 2007.06a
• /
• pp.188-190
• /
• 2007

The MEA with the catalyst layer containing PtRu black and 60 wt. %Pt/C as their anode and cathode catalysts. For find to effect of carbon support, the MEA with platinum black for cathode catalyst was fabricated. The performance of the MEA with the catalyst layer containing (PtRu black:60 wt.% Pt/C) as their anode and cathode catalyst has shown competitively higher value than the performance of the MEA with the catalyst layer containing (PtRu black:Pt black) as their anode and cathode catalyst.

• CELLMED
• /
• v.4 no.3
• /
• pp.18.1-18.5
• /
• 2014

Leea asiatica (L.) Ridsdale, a folk medicinal plant is used by the ethnic people of North East India for the treatment of hepatic disorder. In this study, we have investigated the hepatoprotective and antioxidant activity of L. asiatica leaves against acetaminophen induced hepatotoxicity. Methanol extract of L. asiatica (150 and 300 mg/kg/day, p.o.) were administered to rats for three consecutive days followed by single acetaminophen (3000 mg/kg, p.o.) administration on $3^{rd}$ day. After 48 h of acetaminophen administration animals were sacrificed and biochemical estimation of serum, in vivo antioxidant activity using liver tissue were carried out. High levels of serum glutamate oxaloacetate transaminase, serum glutamate pyruvate transaminase, serum alkaline phosphatase, total bilirubin, direct bilirubin, total cholesterol and triglycerides were observed in disease control group, which found near to normal in extract treated groups. Higher dose exhibited significant hepatoprotective activity against acetaminophen induced toxicity. Level of superoxide dismutase, catalase, glutathione peroxidase in liver tissue, and reduced glutathione in liver and blood were also significantly increased in extract (300 mg/kg) treated animals compare to disease control group. In this study we found that leaves of L. asiatica exhibited potent hepatoprotective activity against acetaminophen induced hepatic damage in experimental animals which justify the folklore claim, and the possible mechanism of this activity may be due to strong antioxidant activities of extract.