• Bulletin of the Korean Chemical Society
• /
• 제32권12호
• /
• pp.4337-4340
• /
• 2011

The vitamin D receptor binding peptide, VDRBP, was overexpressed as a fused form with the ubiquitin molecule in Rosetta(DE3)pLysS, a protein production strain of Escherichia coli harboring an induction controller plasmid. The fusion protein was bound to the immobilized metal ions, and the denaturation and renaturation of the fusion protein were performed as a part of the purification procedure. After the elution of the fusion protein, the peptide hormone was released from its fusion partner by using yeast ubiquitin hydrolase (YUH), and subsequently purified by reverse phase chromatography. The purity of the resulting peptide fragment was checked by MALDI-TOF mass and NMR spectroscopy. The final yields of the target peptide were around 5 and 2 mg per liter of LB and minimal media, respectively. The recombinant expression and purification of this peptide will enable structural and functional studies using multidimensional NMR spectroscopy and X-ray crystallography.

• 약학회지
• /
• 제36권3호
• /
• pp.205-211
• /
• 1992

A simple dignostic method using Fast Atom Bombardment mass spectrometry was applied to the characterization of green tea flavonols from the eluates of Sepahadex LH-20 column chromatography. From the ethyl acetate extracts, crude mixture of flavonol fraction(Fr.$1{\sim}4$) were separated by the stepwise gradient elution with 30, 45, and 60% aqueous acetone. Procyanidine B analogues were found to be typical constituents of Fr. 1. Main components of Fr. 2 were catechins and gallo-catechins. Fr. 3 contained mainly ester type compounds, catechin-gallates, gallocatechin-gallates with their analogues. Fr. 4 was contaminated with some phthalate esters.

• 환경위생공학
• /
• 제12권1호
• /
• pp.15-23
• /
• 1997

The anionic exchange resins with the Dowex-1 and Amberlite CG-400 form were transformed into resin of sulfate and acetate acid form, respectively. The uranyl complex ions with SO$_{4}$$^{2-}$ and CH$_{3}$COO$^{-}$ were adsorbed on the anion exchange resion mentioned above, and these complex ions were eluted as mixture eluents of 0.7M HNO$_{3}$ - 0.5M NH$_{4}$NO$_{3}$ by anion exchange chromatography. The optimum adsorption conditions of uranyl anion complex ions adsorbed on the upper of the resin colmun were 1.5-2.0 ml/min of flow rates at pH 2.0 and adsorptive power of uranyl complex ion of sulfuric acid type were nearly consistent with the Caussion normal distribution curve, whereas the elution state of UO$_{2}$(Ac)$_{2}$$^{4-}$ with acetic acid type was departed. The weighing form obtained from resin of sulfuric acid and aceric acid type was U$_{3}$O$_{8}$ whose recovery was 91.7%. The possibility of recovering uranium from the monazite sulfate solution using a strong base anion resin, Amberlite CG-400(sulfate form), was successfully recovered more than 90%.

• Asian-Australasian Journal of Animal Sciences
• /
• 제1권2호
• /
• pp.99-106
• /
• 1988

A high performance liquid chromatographic procedure is described for the direct determination of the picomole amount of palmitoyl-Coenzyme A and stearoyl-Coenzyme A, using a stainless steel column packed with C-18 derivatized porous silica ($5{\mu}m$), an isocratic elution with a mixture of 33 mM $KH_2PO_4$/acetonitrile as a mobile phase and a UV detector. The long-chain acyl-Coenzyme A esters were determined in incubated microsomal fractions of a bovine liver to demonstrate the utility of this method for monitoring acyl-CoA synthesis in biological samples. The reaction rate of palmitate was higher than that of stearate. After a 60 minute incubation period, the generated amount of palmitoyl-Coenzyme A and stearoyl-Coenzyme A were approximately 70 and 20 n mol/mg micresomal protein, respectively. The advantage of this method are in that no decomposition of the CoA esters is involved, while the constituent molecular species is detected.

• Natural Product Sciences
• /
• 제9권2호
• /
• pp.45-48
• /
• 2003

The content of chiisanoside in the Acanthopanax Species was determined by reversed-phase high performance liquid chromatographic method. Chiisanoside was separated from the other components in the plant extracts using Zorbax 300 SB $C_{18}$ column with gradient elution of acetonitrile. Identification of chiisanoside was carried out by comparison in the LC/MS spectrum of separated peak from extract with that of standard. By HPLC analysis in this experiment, Acanthopanax species could be classified into two groups based upon the content of chiisanoside-one with low concentration of chiisanoside, such as A. senticosus and A. koreanum, and another with high concentration of chiisanoside, such as A. senticosus f. inermis, A. Divaricatus var. albeofructus, and A. chiisanensis.

• 약학회지
• /
• 제25권3호
• /
• pp.101-108
• /
• 1981

Quantitative determination of capsaicin in biological fluid was investigated. The pharmacokinetic study of capsaicin in rabbits was performed by high-pressure liquid chromatography, equipped with a microparticulate reversed-phase column and a fixed wavelength detector. Elution was carried out using methanolwater(70:30). It allows the quantitative determination at 8-400 ng level. When single dose of capsaicin(4mg/kg) was given to rabbits intravenously, the elimination phase was extremely short with average half-life to 17.35 minute. Urine excretion of capsaicin itself during first 2 hours after intravenous administration (4mg/kg) was 0.004-0.04% of the administered amount. The maximum plasma concentration of capsaicin after oral administration (300mg/kg) was $4{\times}10^{-7}$g/ml at 40 minutes. The $LD_{50}$ of capsaicin in mouse was 0.40mg/kg (i.v.) and 47.2 mg/kg (p.o.) which was determined by Litchfield and Wilcoxon's method, suggesting that the gastrointestinal absorption of capsaicin is poor.

• 약학회지
• /
• 제29권6호
• /
• pp.375-379
• /
• 1985

The gas chromatographic behavior of optically active N-(N-benzoyl-L-valyl)-anilide used as stationary phase is described. N-(N-benzoyl-L-valyl)-anilide has been synthesized with good yield under mild condition via Schotten-Bauman process and coated on the Chromosorb W AW (80-100mesh) for the purpose of enantiomer separation. The behavior of this compound as optically active stationary phase for the separation of the enantiomers of N-TFA-D, L-amino acid isopropyl esters has been examined with respect to the correlation between the separation factors and column temperatures. All amino acid enantiomers examined were eluted within one hour and the elution pattern showed retention times increasing in the order of alanine, valine, leucine, threonine, proline and methionine.

• 대한화학회지
• /
• 제18권5호
• /
• pp.358-362
• /
• 1974

벤조산과 그 유도체들에 대한 음이온 교환분리를 여러 농도의 염화니켈-메탄올 용매 내에서 연구하였다. Amberlite CG-400, $Cl^-$ form에 대한 유기산들의 부피분배계수를 측정하고 이 분배계수로부터 제시된 적절한 농도의 $NiCl_2-MeOH$ 용액을 용리액으로 사용하여 몇 개의 혼합유기산을 정량적으로 분리하였다. 모든 유기산들의 농도는 자외선 분광광도계를 사용하여 정량하였다.

• Journal of Pharmaceutical Investigation
• /
• 제16권3호
• /
• pp.106-109
• /
• 1986

The elution of di(2-ethylhexyl) phthalate (DEHP) from flexible bags into human blood or transfusion was studied. The conditions of determination of DEHP using high performance liquid chromatography (HPLC) was established as follows: Condition I-column, ${\mu}-Bondapak^{TM}\;C_{18}$; mobile phase, methanol: water=91 : 9 ; flow rate, 1.2ml/min; wavelength, 254nm; injection volume, $10{\mu}l$. Condition II-column, Lichorsorb RP-18$(10{\mu}m)$; mobile phase, methanol: water=94 : 6 ; flow rate, 1.1ml/min; wavelength, 254nm; injection volume, $10{\mu}l$. DEHP was found to be migrating from PVC blood and total parentral nutrient bags into methanol, but not into anti, coagulant drug solution.

• 한국안전학회지
• /
• 제11권4호
• /
• pp.84-89
• /
• 1996

The Oxidation of aflatoxin $G_1$ ($AFG_1$) with ozone in chloroform solvent gave the stable ozonide into ozonization of the double bond in the terminal furan ring, and this reaction have been carried out for 3hr at -78. 5$^{\circ}C$. The chloroform solvent was removed in a stream of nitrogen and the residue was separated by elution chromatography(EC). The structure of this compound have been identified by using MS, $^1H-NMR$, $^l3C-NMR$ and I. R spectroscopy, respectively. This compound was formed the normal stable AFG$_1$-ozonide into spontaneous rearrangement after unstable ozonide according to sigmatropic rearrange ment dependent upon cyclo addition by ozone.