During the initial cooling period of spent nuclear fuel, Cs-137 and Sr-90 constitute a large portion of the total decay heat. Therefore, separating cesium and strontium from spent nuclear fuel can significantly decrease decay heat and facilitate disposition. This study presents analytical technique based on the gas pressurized extraction chromatography (GPEC) system with cation exchange resin for the separation of Sr, Cs, and Ba. GPEC is a micro-scaled column chromatography system that allows for faster separation and reduction volume of elution solvent compared to conventional column chromatography by utilizing pressurized nitrogen gas. Here, we demonstrate the comparative study of the conventional column chromatography and the GPEC method. Cation exchange resin AG 50W-X12 (200~400 mesh size) was used. The sample was prepared at a 0.8 M hydrochloric acid solution and gradient elution was applied. In this case, we used the natural isotopes 88Sr, 133Cs, and 138Ba instead of radioactive isotopes for the preliminary test. Usually, cesium is difficult to measure with ICP-OES, because its wavelengths (455.531 nm and 459.320 nm) are less sensitive. So, we used ICP-MS to determine the identification and the recovery of eluate. In this study, optimized experimental conditions and analytical result including reproducibility of the recovery, total analysis time and volume of eluents will be discussed by comparing GPEC and conventional column chromatography.

This study was performed to evaluate the separation of Sr, Cs, Ba, La, Ce, and Nd using gas pressurized extraction chromatography (GPEC) with anion exchange resin for the quantitation of Neodymium. GPEC is a micro-scaled column chromatography system that provides a constant flow rate by utilizing nitrogen gas. It is overcome the disadvantages of conventional column chromatography by reducing the volume of elution solvent and shortening the analysis time. Here, we compared the conventional column chromatography and the GPEC method. The whole analysis time was decreased by nine times and radioactive wastes were reduced by five times using the GPEC system. Anion exchange resin 1-X4 (200~400 mesh size) was used. The sample was prepared at a 0.8 M nitric acid in methanol solution. The elution solvent was used at a 0.01 M nitric acid in methanol solution. Finally the eluate was analyzed by ICP-MS to determine the identification and recovery. In this case, we applied the natural isotopes of LREEs (139La, 140Ce, and 144Nd) and high activity nuclides (88Sr, 133Cs, and 138Ba) instead of radioactive isotopes for the preliminary test; as a result, unnecessary radioactive waste was not produced. The recoveries were 93.9%, 105.9%, 91.9%, 47.6%, 35.9%, and 79.9% of Sr, Cs, Ba, La, Ce, and Nd, respectively. The reproducibility of recoveries by GPEC were in the range 2.8%–10.9%.

A new method for chemical separation of light rare-earth elements (LREEs) using gas-pressurized extraction chromatography (GPEC) is described. GPEC is a microscale column chromatography system that features a constant flow of solvents (0.1 mL/min), which is created by pressurized nitrogen gas. The separation column with a Teflon tubing was packed with LN resin. We evaluated the separation of Ba, La, Ce, and Nd using various elution solvents. Here, we applied the natural isotopes of LREEs (La-139, Ce-140, and Nd-144) and barium (Ba-138) instead of radioactive isotopes for the preliminary test and reducing unnecessary radioactive waste. The column reproducibility of the proposed GPEC system ranged from 2.4% to 4.9% with RSDs of recoveries, and the column-to-column reproducibility ranged from 3.1% to 6.3% with RSDs of recoveries. This proposed GPEC method provides robust analysis and facilitates production of lesser chemical wastes and faster separation owing to the use of low solvent volume compared to traditional column chromatography.

재조합 β-galactosidase (β-gal) 을 이용하여 transgalactosylation 반응으로 합성된 2-phenoxyethanol galactoside (PE-gal)과 chlorphenesin galactoside (CPN-gal)의 정제를 실시하였다. 먼저 PE와 PE-gal이 포함된 반응물에 ethyl acetate (EA)를 넣고, EA/water 이상계 시스템에서 PE와 PE-gal을 분획하였다. 이 시스템에서 PE는 EA층으로 PE-gal은 water층으로 분획되었다. 그리고, 물층을 모아서 silica gel chromatography를 실시하였다. 최종적으로, silica gel chromatography만 실시하여 PE-gal을 정제한 경우와, EA 처리 후 silica gel chromatography를 실시하여 PE-gal을 정제한 경우의 정제 PE-gal에 대하여 HPLC (High performance liquid chromatography)와 TLC (thin-layer chromatography) 분석을 수행하였다. 그 결과 EA를 처리하여 분획한 후, silica gel chromatography를 수행한 시료에서 잔여 PE가 완전히 제거되는 것을 관찰하였고, silica gel chromatography만 실시하여 PE-gal을 정제한 경우에는 상당량의 잔여 PE가 관찰되었다. 이 때, mole 기준으로 약 21%의 정제 수율을 확인할 수 있었다. 마찬가지로 CPN-gal의 정제에서도 EA 분획 처리 후, silica gel chromatography를 수행하였더니, 잔여 CPN이 거의 없는 순수한 CPN-gal을 얻을 수 있었다.

선행연구에서 화장품 소재로서 보습력과 방부력을 가지고 있는 1, 2-hexanediol (HD)의 transgalactosylation 반응을 통하여 galactose한 분자가 HD에 결합한 1, 2-hexanediol galactoside (HD-gal)의 합성을 확인하였다. 본 연구에서 재조합 β-galactosidase (β-gal)가 발현된 Escherichia coli (E. coli) 세포를 이용하여 약 94%의 수율로 HD-gal가 합성되는 것을 관찰하였고, HD-gal을 합 성한 후, 보다 효과적인 HD-gal의 정제 방법에 대하여서도 연구하였다. 먼저 고농도의 lactose (300 g/l) 존재 하에서 β-gal을 함유한 E. coli 세포를 이용하여, 48 시간 동안 75 mM의 HD로 부터 HD-gal이 합성되는 것을 TLC 분석으로 확인하였고, 반응액에서 E. coli β-gal의 존재를 Western blotting으로 확인할 수 있었다. HD-gal을 효과적으로 순수 정제하기 위하여, 용매를 사용하여 transgalactosylation 반응이 끝난 후 잔여 HD를 우선 제거하고, 이어서 silica gel chromatography를 수 행하는 방법을 실시하였다. 물에 녹지 않는 용매로는 methylene chloride와 ethyl acetate를 선택하여 비 교 실험하였는데, ethyl acetate를 사용하여 4회 물층을 분획하여, 잔여 HD를 효과적으로 제거할 수 있 었다. 그 후, 이어서 silica gel chromatography 수행하여, 순수한 HD-gal을 효과적으로 정제하였다. 반 응에 첨가된 75 mM의 HD를 기준으로 최종 정제된 HD-gal의 생산 수율은 mole 기준으로는 약 8.9±0.6% (n=3), weight 기준으로 약 21.1±1.4% (n=3) 정도였다. 앞으로 이러한 정제 방법을 이용하 여 얻은 HD-gal의 항균력 변화를 HD와 비교하여 평가할 예정이고, 피부세포에 대한 독성 변화를 역시 HD와 비교하여 분석할 예정이다.

The pomegranate (Punica granatum), especially its fruit, possesses a vast ethnomedical history and represents a phytochemical reservoir of heuristic medical value. The tree and fruit can be divided into several anatomical compartments, and the fruit juice, peel and oil are known to be weakly estrogenic and heuristically of interest for treatment of menopausal symptoms and sequellae. In this study, analysis of estrogen in pomegranate extract was carried out with LC/MS/MS. Three batches of pomegranate extract samples were used to analysis the target compounds (estrogen). The contents of estrogen derivatives in the samples were 38.6 ppb of estriol, 83.5 ppb of estrone,and 10.9 ppb of estradiol. This result suggests that the pomegranate extract can used for treatment of menopause symptoms in the woman.

A rapid and simple method for the quantitative determination of volatile fatty acids (VFAs; propionic acid, n-butyric acid, i-valeric acid and n-valeric acid) and indoles (phenol, p-cresol, 4-ethyl phenol, indole and skatole) in pig slurry and dog excrement using solid-phase micro-extraction (SPME) coupled to gas chromatography was evaluated. 50/30 ㎛ DVB/CAR/PDMS (Divinylbenzene/Carboxen/Polydimethylsiloxane) fiber was used to extract the target compounds in aqueous media. Sample amount and adsorption time was standardized for the routine analysis. Detection limits were from 0.11 to 0.15 ㎍/L for VFAs and from 0.12 to 0.28 ㎍/L for indoles and the correlations observed (R2) were 0.975～1.000. This method was applied to the pig slurry, fertilizer, compost and dog excrement. In nearly all cases, the indoles were detected in concentrations of higher than their limits of detection (DOLs). But the VFAs in swine manure were below their DOLs.