• 한국자원식물학회:학술대회논문집
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• 한국자원식물학회 2018년도 추계학술대회
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• pp.92-92
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• 2018

Silene seulensis Nakai was used as traditional medicines in Korea, we collected plant from demilitarized zone (DMZ). S. seulensis was extracted with 30, 50, and 70% ethanol and partitioned successively with n-hexane, EtOAc, dichloromethane and BuOH. These extracts (30, 50 and 70% ethanol) were evaluated the cytotoxicity on B16F10 and Hacat cell lines. The LC-MS/MS data of each fractions (n-hexane, EtOAc, dichloromethane, and BuOH) were compared with MS library, combined with ultraviolet/visual (UV/Vis) and MS data for faster determine structure by database search results. This led to the identification of four compounds (1-4) from S. seulensis. These compounds was isolated first time from S. seulensis. Their chemical structures are elucidated by combinations of NMR and mass spectrometry techniques.

• 대한화학회지
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• 제38권10호
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• pp.726-733
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• 1994

대기부유분진(air particulate material)중에 존재하는 다환방향족탄화수소(polycyclic aromatic hydrocarbons, PAH)를 신속하고 정확하게 분석하기 위하여 대기부유분진 시료를 10ml의 초임계유체($N_2O$ )로 30분간 추출 후 별도의 전처리와 농축과정 없이 GC/MS에서 분석하여 분석시간과 분석과정을 단축 및 단순화하였다. 시료로서 NBS 대기부유분진 인증표준기준물질(certified particulate reference material, CRM)1649와 서울의 도심에서 채취한 대기부유분진 시료를 이용하여 기존의 추출법 및 분석방법과 비교하였다. 그 결과 본 분석방법은 기존의 분석법에 비해 회수율은 상대적으로 작았으나 재현성이 좋았으며 분석과정이 간단하고 분석시간이 현저히 단축됨을 알 수 있었다.

• 한국연초학회지
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• 제36권1호
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• pp.12-19
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• 2014

A matrix solid-phase dispersion (MSPD) method was developed for extracting and cleaning-up the selected agrochemicals in tobacco using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS-SIM). Different parameters of the method were investigated and optimized, such as the type of solid-phase (alumina, $C_{18}$ and Florisil) and eluent (acetone, acetonitrile, ethylacetate and n-hexane). The best results were obtained using 0.5 g of tobacco sample, 1.0 g of $C_{18}$ as dispersant sorbent, 1.0 g of Florisil as clean-up sorbent and acetonitile saturated with n-hexane as eluting solvent. The method was validated using tobacco samples fortified with agrochemicals at their different concentration levels. This method gave good linearity for the selected agrochemicals of ranging from $0.01{\mu}g/mL$ to $0.1{\mu}g/mL$. Recoveries of the selected agrochemicals in tobacco were more than 80 % and reproducibilities were found to be better than 10 % RSD. Those results suggested that the analytical procedure including MSPD method in combining with GC/MS could be applicable to the rapid determination often the selected agrochemicals in tobacco.

• Fisheries and Aquatic Sciences
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• 제18권2호
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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.

• 분석과학
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• 제15권3호
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• pp.221-228
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• 2002

MX [3-chloro-4(dichloromethyl)-5-hydroxy-2(5H)-furanone]는 수돗물의 소독을 위해 첨가한 염소와 수중의 유기물이 반응하여 생성되는 강력한 변이원성 물질이다. 본 논문에서는 GC/MS를 이용하여 유도체화 시약인 2% 황산-methanol, iso-propanol, sec-butanol, n-butanol을 이용하여 MX의 유도체화를 비교하였으며, 이온화 방법으로 EI 와 NCI를 비교한 결과, NCI 방법에서 검출 한계가 1.25 pg으로 EI 방법에서는 25 pg이였으며, 25~2500 pg 범위에서 직선성을 나타내었다.

• 공업화학
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• 제7권1호
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• pp.171-176
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• 1996

환경 친화성인 비이온 계면활성제 글루카마이드(N-알킬-N-아실 글루카민)는 크게 두 단계 반응으로 구분되는데, 첫 단계는 알킬 아민과 글루코스를 메탄올 용매하에 아민화 반응시킨 후, Ni 촉매하에 고압으로 환원시킨 결과 4종의 알킬 글루카민을 86~93%의 수율로 얻었다. 2단계 반응에서는 4종의 알킬 글루카민과 4종의 지방산 메틸 에스테르를 알칼리 촉매하에 메탄올을 환류시키면서 합성한 결과 16종중 12종의 글루카마이드는 84~95%수준의 높은 수율을 보였으나, 알킬기가 벤질일 경우에는 50~70%의 낮은 수율을 나타내었다. 알킬 글루카민 4종과 글루카마이드 16종에 대한 분자구조 확인은 IR, MS, NMR로 확인하였다.

• Elastomers and Composites
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• 제43권1호
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• pp.31-38
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• 2008

[ $FeCl_3$ ]를 첨가한 초음파 조건에서 4-nitroaniline, 3-nitroaniline, and 4-isopropylaniline등의 방향족 아민 화합물과 풀러렌 산화물$[C_{70}(O)_n](n\geq1)$을 반응시켰다. 이 반응은 방향족 아민 화합물을 사용한 풀러렌 산화물 쪼개짐 반응이다. MALDI-TOF-MS and UV-vis spectra를 사용하여 생성된 화합물이 아민화 풀러렌 유도체임을 확인하였다.

• Molecules and Cells
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• 제25권1호
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• pp.43-49
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• 2008

Cancer Osaka thyroid, also known as Tpl-2 (Cot) is a member of the MAP3K kinase family and plays a key role in the regulation of the immune response to pro-inflammatory stimuli such as lipopolysaccharide (LPS) and tumour necrosis $factor-{\alpha}$ ($TNF-{\alpha}$). A series of Cot constructs with an N-terminal 6xHis tag were transiently expressed in HEK293 cells: $Cot_{130-399}$ (kinase domain), $Cot_{1-388}$ (N-terminal and kinase do-mains), $Cot_{1-413}$, $Cot_{1-438}$ (containing a putative PEST sequence), $Cot_{1-457}$ (containing both PEST and degron sequences) and $Cot_{1-467}$ (full-length protein). These Cot proteins were pulled down using an anti-6xHis antibody and separated by 2D electrophoresis. The gels were silver-stained and 21 proteins were detected that did not appear, or had substantially reduced intensity, in the control sample. Three of these were identified by MS and MS/MS analysis as Hsp90, Hsp70 and Grp78. Hsp90 appeared to bind to the kinase domain of Cot and this interaction was further investigated using co-immuno-precipitation with both overexpressed Cot in HEK293 cells and endogenous Cot in Hela cells.

• Natural Product Sciences
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• 제16권3호
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• pp.164-168
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• 2010

High-performance liquid chromatographic method with diode-array detector and electrospray ionization with multi-stage tandem mass spectroscopy (HPLC/DAD/ESI-$MS^n$) was used to identify the major constituents in a methanolic extract of Eclipta prostrata. The chromatographic separation was performed on a C18 column. Acetonitrile-water was used as a mobile phase. HPLC/DAD/ESI-$MS^n$ allowed the characterization of constituents of E. prostrata, mainly triterpenoids (eclalbasaponin I, II, III, IV, VI), flavonoids (luteolin 7-O-glucoside, demethylwedelolactone, wedelolactone, luteolin, demetylwedelolactone sulfate, luteolin sulfate, apigenin sulfate) and phenolic acids (5-O-caffeoylquinic acid, 3, 4-O-dicaffeoylquinic acid, 3, 5-O-dicaffeoylquinic acid, 4, 5-Odicaffeoylquinic acid).

• 한국수산과학회지
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• 제53권2호
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• pp.174-180
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• 2020

The mouse bioassay has been used widely for the monitoring of paralytic shellfish toxins (PSTs) in many countries. However, this method shows low sensitivity and high limit of detection (LOD), as well as it cannot confirm toxic profiles. Recently, LC-MS/MS method was studied for the quantitative of PSTs, however, the method has any problems with unstable retention times by ionization suppression caused by high salt concentration in shellfish extracts. To establish an alternative method for PSTs analysis, we tried to original LC-MS/MS methods adding desalting operation using amorphous graphitized polymer carbon solid-phase extraction cartridges. The method validation was conducted to determine linearity, limit of detection, limit of quantification (LOQ), accuracy, and precision in quantifying PSTs. The correlation coefficients for all tested PSTs maintained over 0.999. The LODs and LOQs for all PSTs were about 0.19-1.05 ㎍/kg and 0.58-3.18 ㎍/kg, respectively. The accuracies for PSTs were 95.4-107.7% for saxitoxin group, 97.1-100.9% for gonyautoxin group, 99.0-100.8% for N-sulfocarbamoyl toxin group, and 96.8-104.6% for decarbamoyl toxin group. These results indicate that the modified LC-MS/MS method was appropriate for analyzing the PSTs in shellfish and tunicates.