• 한국산업보건학회지
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• 제7권1호
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• pp.49-59
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• 1997

This study was performed to analyze the purity of technical grade ${\alpha}$-naphthylamine, to establish optimal analytical condition of ${\alpha}$-naphthylamine in urine and to determine the urine sample of workers exposed to ${\alpha}$-naphthylamine. The purity of technical grade ${\alpha}$-naphthylamine were $96.5{\pm}2.38%$, $94.1{\pm}0.97%$, $97.0{\pm}0.02%$ by gas chromatography-mass selective detector. To analyze ${\alpha}$-naphthylamine in urine, high performance liquid chromatography-electrochemical detector and gas chromatography-electron capture detector operating conditions have been optimized by preliminary expriment. In high performance liquid chromatography-electrochemical detector, the mobile phase was consisted of acetonitrile(35%) and water(65%), and the flow rate was maintained at 1.0ml per minute. Optimal detective condition was 9.0V(10nA/V) of electrochemical detector. The recovery of sep-pak treatment method was highly estimated as pretreatment of ${\alpha}$-naphthylamine in urine. The free amine was isolated by gas chromatography-electron capture detector after basic hydrosis, sep-pak treatment, toluene elution and HFBA(heptafluoro-butyric anhydride) derivatization of urine. The recovery of ${\alpha}$-naphthylamine in urine was $98.73{\pm}3.29%$ by gas chromatography-electron capture detector. The sensitivity was more higher than that of high performance liquid chromatography-electrochemical detector. Urinary ${\alpha}$-naphthylamine was detected in only one worker among nine workers. The level of ${\alpha}$-naphthylamine in urine was 6.42 ng/ml.

• Bulletin of the Korean Chemical Society
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• 제25권12호
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• pp.1833-1839
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• 2004

Recently mass spectrometry and separation methods such as liquid chromatography have become major tools in the field of proteomics. In this report, we describe in detail our efforts to develop ultra-high pressure capillary reverse-phase liquid chromatography (cRPLC) and its online coupling to a mass spectrometer by a nanoelectrospray (nanoESI) interface. The RPLC system is constructed in house to deliver LC solvents at the pressure up to 20,000 psig, which is four times higher than conventional RPLC systems. The high operation pressure allows the efficient use of packed micro-capillary columns (50, 75 and 150 ${\mu}$m i.d., up to 1.5 m long). We will discuss the effect of column diameter on the sensitivity of cRPLC/MS/MS experiments and the utility of the developed technique for proteome analysis by its application in the analysis of proteome samples having different levels of complexity.

• Journal of Applied Biological Chemistry
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• 제58권1호
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• pp.9-11
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• 2015

Tissue extracts were prepared from liquid-cultured Arabidopsis and reacted with UDP-[$^3H$]-GlcNAc. Phospholipid fractions were then extracted by butanol partitioning. Consecutive thin-layer chromatography identified two glycolipids sensitive to PI-specific phospholipase C, known as early intermediates in glycosylphosphatidylinositol anchor biosynthesis; phosphatidylinositol N-acetylglucosamine and phosphatidylinositol glucosamine.

• Bulletin of the Korean Chemical Society
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• 제26권4호
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• pp.569-574
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• 2005

A coupled column liquid chromatography system was applied for the separation of the burnup monitors in spent nuclear fuel sample solutions. A reversed phase column was studied for the adsorption behavior of uranyl ions using alpha-hydroxyisobutyric acid as an eluent and used for the separation of plutonium and uranium. A cation exchange column prepared by coating 1-eicosylsulfate onto the reversed phase column was used for the separation of the lanthanides. In addition, retention of Np was checked with the reversed phase column and cation exchange column, respectively, according to the oxidation states to observe the interference effect for the separation of burnup monitors. This chromatography system showed a great reduction in separation time compared to a conventional anion exchange method. A good agreement from the burnup data was obtained between for this method and a conventional anion exchange method to within 1% of a difference for the spent nuclear fuel samples of about 40 GWD/MTU.

• Natural Product Sciences
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• 제21권2호
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• pp.111-121
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• 2015

The root of Panax ginseng, is a Korea traditional medicine, which is used in both raw and processed forms due to their different pharmacological activities. As part of a continued chemical investigation of ginseng, the focus of this research is on the isolation and identification of compounds from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, semi-preparative-high performance liquid chromatography, Fast atom bombardment mass spectrometric, and nuclear magnetic resonance. Dammarane-type triterpenoid saponins were isolated from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, and semi-preparative-high performance liquid chromatography. Their structures were identified as protopanaxadiol ginsenosides [gypenoside-V (1), ginsenosides-Rb1 (2), -Rb2 (3), -Rb3 (4), -Rc (5), and -Rd (6)], protopanaxatriol ginsenosides [20(S)-notoginsenoside-R2 (7), notoginsenoside-Rt (8), 20(S)-O-glucoginsenoside-Rf (9), 6-O-[$\alpha$-L-rhamnopyranosyl(1$\rightarrow$2-$\beta$-D-glucopyranosyl]-20-O-$\beta$-D-glucopyranosyl-$3\beta$,$12\beta$, 20(S)-dihydroxy-dammar-25-en-24-one (10), majoroside-F6 (11), pseudoginsenoside-Rt3 (12), ginsenosides-Re (13), -Re5 (14), -Rf (15), -Rg1 (16), -Rg2 (17), and -Rh1 (18), and vinaginsenoside-R15 (19)], and oleanene ginsenosides [calenduloside-B (20) and ginsenoside-Ro (21)] through the interpretation of spectroscopic analysis. The configuration of the sugar linkages in each saponin was established on the basic of chemical and spectroscopic data. Among them, compounds 1, 8, 10, 11, 12, 19, and 20 were isolated for the first time from P. ginseng root.

• 한국식품과학회지
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• 제30권6호
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• pp.1247-1251
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• 1998

식초의 에탄올과 초산을 동시에 분석하고자 packed column으로 gas chromatographic analysis을 모색하였다. Tenax-GC를 충진물로 사용하여 $2\;m{\times}2\;mm$의 stainless steel column을 제조하고 식초를 여과하여 column에 직접 주입한 결과 내부 표준 물질로 사용한 isopropyl alcohol과 에탄올, 초산이 20분 이내에서 완전히 분리되었으며 정확도가 매우 높은 것으로(P<0.05)나타났다. 19종의 식초를 이용하여 적정방법으로 산도를, packed column GSC로 에탄올과 초산을, HPLC로 초산을, capillary column GLC로 에탄올과 초산을 각각 분석하여 분석치들을 상호 비교하였다.

• 한국자기공명학회논문지
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• 제15권1호
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• pp.14-24
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• 2011

We have performed Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) analysis for liquid crystalline mixture and elucidated the structures of selected components by NMR spectra. Combining the results of one-dimensional 1H experiments as well as homonuclear and heteronuclear two-dimensional experiments, we could analyze the molecular structure of the liquid crystal singles whose structure had not been interpretable by mass spectrometry alone.

• Mass Spectrometry Letters
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• 제8권4호
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• pp.90-97
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• 2017

Androgenic anabolic steroids (AASs) are synthetic derivatives of testosterone with a common structure containing cyclopentanoperhydrophenanthrene nucleus. Their use enhances the muscle building capacity and is beneficial during performance. The AASs are one of the most abused group of substances in horse doping. Liquid chromatography tandem mass spectrometry ($LC/MS^n$) has been successfully applied to the detection of anabolic steroids in biological samples. However, the saturated hydroxysteroids viz: nandrolone, $5{\alpha}-estrane-3{\beta}$, $17{\alpha}-diol$ exhibit lower detection responses in electrospray ionisation (ESI) because of their poor ionisation efficiency. To overcome this limitation pre-column chemical derivatization has been introduced to enhance their detection responses in $LC-ESI-MS^n$ analysis. The aim of present study was to develop a sensitive method for identification and confirmation of nandrolone and its metabolite in horse urine incorporating pre-column derivatization using picolinic acid. The method consists of extraction of targeted steroid conjugates by solid phase extraction (SPE). The eluted steroid conjugates were hydrolysed by methanolysis and free steroids were recovered with liquid-liquid extraction. The resulting steroids were derivatized to form picolinoyl esters and identification was done using LC-ESI-MS/MS in positive ionization mode. The picolinated steroid adduct enhanced the detection levels in comparison to underivatized steroids.

• Food Science and Biotechnology
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• 제18권4호
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• pp.978-984
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• 2009

An analytical method for the simultaneous determination of 9 quinolones (QNs) in porcine, chicken, and bovine muscles was developed and validated using liquid chromatography-fluorescence detector (LC-FLD). The samples were extracted using a liquid-liquid extraction (LLE) process. Chromatographic separation was achieved on a reverse phase $C_8$ column with a gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and acetonitrile (ACN). The proposed method was validated according to the Food and Drug Administration (FDA) guideline for bioanalytical assay procedures. Recoveries of QNs were 83.1-111.9% with relative standard deviations (RSDs) below 15%. Linearity within a range of 30-500 ${\mu}g/kg$ was obtained with the correlation coefficient ($R^2$) of 0.9967-0.9999. The limits of detection (LOD) were 1-16 ${\mu}g/kg$. These values were lower than the maximum residues limits (MRLs) established by the European Union (EU). The present method was successfully applied to determine QNs in edible muscles.

• 분석과학
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• 제6권3호
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• pp.267-274
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• 1993

두 가지 파라미터를 이용한 반복 회귀 최적화법을 미셀 액체 크로마토그래피에서 아미노산과 팹티드류의 분리에 적용하였다. 실험에 사용한 파라미터들은 계면활성제(surfactant)인 SDS와 2-propanol의 농도이다. 이 최적화 방법은 작은 횟수의 초기 실험 수행으로 효과적인 최적화점을 얻을 수 있었다.