• Analytical Science and Technology
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• v.31 no.1
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• pp.23-30
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• 2018

Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

• Korean Journal of Food Science and Technology
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• v.31 no.2
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• pp.285-292
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• 1999

An analytical method applicable to quality control and its optimum conditions were studied for rapid and efficient analysis of sorbic and benzoic acids used as preservatives in the commercial soybean paste. In gas chromatographic analysis of sorbic and benzoic acids, the application of HP-FFAP (acid modified polyethylene) wide bore column improved the separation ability significantly. By setting the oven temperature of GC to $200^{\circ}C$, the total elapsed time for quantitative analysis was also reduced to the level required in using packed column. By extracting sorbic and benzoic acids from soybean paste with an automatic steam distillation device, the elapsed time for analysis was reduced by 80% more compared to using conventional steam distillation method. The recoveries of sorbic and benzoic acids by the automatic steam distillation were 98.1% and 99.9%, respectively. The sorbic acid was found in 3 samples of 14 commercial soybean pastes, of which contents were $466{\sim}530ppm$, while $0.3{\sim}4.4ppm$ of benzoic acid was found in all the samples.

• Analytical Science and Technology
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• v.12 no.5
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• pp.408-414
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• 1999

A selective and sensitive method for the derivatization of total homocysteine (Hcy) and the related compounds in plasma by gas chromatograph (GC)-electron capture detector (ECD) has been developed. To determine total homocysteine, cysteine (Cys), and methionine (Met) in human plasma using GC-ECD, analytes were reduced and converted into their N(O,S)-ethylearbonyl pentafluoropropyl (PFP) ester by derivatization with ethyl chloroformate and pentafluoropropyl alcohol (PFP-OH) in plasma. The best derivatizing agent N(O,S)-ethyl carbonyl PFP ester, was chosen by comparing the sensitivity of derivatized analysis in GC-ECD. The derivatized analytes in plasma were extracted by chloroform, and subsequently back-extracted with hexane and analyzed by GC-ECD. The calibration carves ($R^2$ > 0.990) were linear over the range $5-50{\mu}mol/L$ of Hcy and Met, $40-400{\mu}mol/L$ of Cys spiked in plasma. The detection limit observed by the established method was below $0.5{\mu}mol/L$. This method is highly sensitive and specific in the analysis of Hcy, Cys, and Met. Therefore, we suggest that this method is appropriate in the analysis of trace concentration of Hcy, Cys, and Met in biological fluids.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.3 no.4
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• pp.309-317
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• 2005

A study on the separation of $^{99}Tc,\;^{94}Nb,\;^{55}Fe,\;^{90}Sr\;and\;^{59/63}Ni$ in various radioactive wastes discharged from nuclear power plants has been performed for a use in their quantification which is indispensible for the evaluation of the radionuclide inventory Ni was recovered along with Ca, Mg, Al, Cr, Ti, Mn, Ce, Na, K, and Cu through the sequential separation procedure of Re(as a surrogate of $^{99}Tc$), Nb, Fe and Sr by anion exchange and Sr-Spec extraction chromatography. In this research, chemical separation of Ni from the co-existing elements was investigated by cation exchange and Ni-Spec extraction chromatography. Precipitation behaviour of Ni and the co-existing elements with dimethylglyoxime(DMG) was investigated in ammonium $citrate/ethanol-H_2O$ and tartaric $acid/acetone-H_2O$ in order to purify separated Ni fractions and to prepare $^{59/63}Ni$ source for the radioactivity measurement using a gas proportional counter. Recovery of Ni separated through ion exchange chromatographic separation procedure was $92.1\%$ with relative standard deviation of $0.9\%$. In addition, recovery of Ni with DMG in the tartaric $acid/acetone-H_2O$ was $85.6\%$ with relative standard deviation of $1.9\%$.

• Korean Journal of Food Science and Technology
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• v.39 no.2
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• pp.122-127
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• 2007

In this study, an analytical method was optimized for detecting dioxin-like PCBs in fish and shellfish. Here, homogenized samples were extracted using an accelerated solvent extraction (ASE) system with 33 mL cell size. Multilayer column chromatography, which consisted of acidic, basic and neutral silica gels, was used for the clean up of the extracts. The instrumental analysis was executed by HRGC/HRMS to a resolution of 10,000 using 4 window multiple ion detection (MID) mode. For the results, the average recoveries ranged from 94.1 to 104.1% (${\pm}8.4$) and the limit of detection was approximately 0.1 pg/g at S/N ratio >3. Finally, the detected concentrations of dioxin-like PCBs for fish and shellfish were in the range of 0.030-1.836 pg TEQ/g.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.3 no.1
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• pp.1-7
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• 2005

Anion exchange chromatography and HDEHP extraction chromatography using DTPA-lactic acid as an eluent were applied in series for the separation of $^{241}$Am and $^{244}$Cm in radwaste samples. The separated elements were determined by electrodeposition at the sodium hydrogen sulfate-sodium sulfate buffer solution followed by alpha-spectrometry. The recovery yields of $^{241}$Am and $^{244}$Cm were 85.2$\pm$$15.3\%$, respectively, from the synthetic solution of spent nuclear fuel sample. The amounts of 241Am and 2440m determined in radwaste sample solutions of condensate bottoms were at the range of 1.5-1.9 Bq/g and -1.7 Bq/g, respectively.

• Applied Chemistry for Engineering
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• v.8 no.2
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• pp.286-291
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• 1997

Taxol which is recognized as a powerful anticancer reagent was extracted from yew extract and separated by NP-HPLC (Normal-PhaseHigh Performance Liquid Chromatography). The experiments were performed in the isocratic mode with $5{\mu}l$ to $100{\mu}l$ injection volume and 1ml/min mobile phase flow rate. The major mobile phase was hexane and small amounts of ethanol, methanol, 1-propanol and isopropanol were added to change the retention behavior. Prior to a real sample, the artificial mixture of taxol, cephalomannine and 10-deacetyltaxol was tested. They are hard to be separated because of similar chemical structures. The experimental results showed that the proper composition of mobile phase for separating the three components was found 96% hexane and 4% ethanol(vol.%) or 96% hexane, 2% 1-propanol and 2% methanol(vol.%). Compared to the run time of 80 minutes for the binary system, the mixture was separated within 50 minutes with the less amount of mobile phase for the ternary system. Finally, $1{\mu}g$ of taxol was separated from yew tree extracts under the optimum operating conditions.

• Analytical Science and Technology
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• v.26 no.4
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• pp.256-261
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• 2013

The efficiency of the two extractions (refluxing extraction and heating-block extraction) was compared to develop the simple analytical method for the determination of capsaicinoids, including capsaicin and dihydrocapsaicin in red pepper powder. For the method development, the parameters, including particle size, extraction time and sample size, were evaluated using ultra high performance liquid chromatography (u-HPLC). It was found that the most effective extraction time of the refluxing extraction was 3 hr. The higher extraction efficiency was obtained with the fine particle of a mild red pepper powder, while the particle size did not affect the extraction efficiency in case of the hot red pepper powder. The higher extraction efficiency was obtained with the small size of sample taken because of the ratio of the large extracting solvent to sample amount. The extraction efficiency of the refluxing method was 3-9% higher than that of the heating-block method, however, the heating-block method could be applied to the determination of capsaicinoids in the red pepper powder for the purpose of quality control of the product.

• Analytical Science and Technology
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• v.20 no.2
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• pp.91-108
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• 2007

This study was investigated both the Korean official soil test method and the international various methods for PCBs in soil sample. The analytical guideline of PCBs in contaminated soil were proposed based on the official soil test methods by discussing the extraction, column cleanup, instrumental conditions, quantification methods of peak matching and individual isomers. The total 28 soil samples were selected by consideration of PCBs-contamination, land use etc., and then analyzed using gas chromatography/electron capture detection (GC/ECD) and gas chromatography/mass spectrometry(GC/MS). In this study, the PCBs were not detected as peak matching method using GC/ECD, but PCBs detected $0.002{\sim}0.487{\mu}g/kg$ using GC/MS in background concentrations.

• Korean Journal Plant Pathology
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• v.12 no.1
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• pp.72-79
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• 1996

보리로부터 분리한 Fusarium sp. BYA-1균주의 감자한천배지 배양체로부터 여러 식물병원곰팡이에 길항력을 나타내는 세 개의 항생물질을 분리하였다. 추출한 세 개의 항생물질은 silica gel관 크로마토그래피와 분취 HPLC, 그리고 Phytolhthora capsici 검정을 이용하여 정제하였다. 이들 분리한 항생물질들을 동정하기 위하여 융점 결정, 자외선흡광법, 질량분석 및 핵자기공명법 등의 기기분석을 실시하였다. 그 결과, 세 개의 항진균성 항생물질들은 fusarielin A, enniatin B, 그리고 enniatin B\ulcorner으로 각각 동정되었다. 분리한 세 개의 물질 중 fusarielin A가 공시된 곰팡이에 가장 강한 항균활성을 나타내었으며, 최소저해농도는 40$\mu\textrm{g}$/ml이하였다. Fusarium속 균주가 구조적으로 다른 두 종류의 항진균성 항생물질인 fusarielin A와 enniatins을 동시에 생성한다는 것은 본 논문에서 처음으로 보고하는 것이다.