• Analytical Science and Technology
• /
• v.22 no.4
• /
• pp.345-353
• /
• 2009

The new anti-impotency analogue was identified in food source. Detection of this analogue was accomplished through screening of food samples by liquid chromatography/photodiode array detector. The spectrum pattern of analogue compound was similar to that observed for hongdenafil which was analogue of sildenafil. This new compound was isolated and purified using the liquid-liquid extraction, thin layer chromatography, column chromatography and preparative HPLC. And then those structure were identified using analytical instruments such as HPLC/PDA, LC/MS/MS and NMR. The compound was given a name to oxohongdenafil which was replaced with acetyl oxoethylpiperazinyl residue instead of sulfonyl piperazine group of sildenafil. The regulation for the abovementioned analogue, oxohongdenafil, was established by Standard of Korean food code.

• Food Science and Biotechnology
• /
• v.17 no.3
• /
• pp.475-482
• /
• 2008

Methanol extracts of peanut (Arachis hypogaea L.) pods were chromatographed, which yielded 3 phytochemicals 1-3 including 5,7-dihydroxychromone (1), eriodictyol (2), and 3',4',5,7-tetrahydroxyflavone (3). To confirm the presence of isolated phytochemicals, the pods extracts were performed by high performance liquid chromatography coupled with a photodiode array detector (HPLC-PDA) and a mass spectrometric detector (MSD) with electrospray ionization (ESI). Optimum extraction conditions for phytochemical contents using peanut germplasm were obtained by employing 90% MeOH for 12 hr at room temperature and phytochemicals 1-3 showed significant differences with concentrations of $407.56{\pm}23.35$, $52.92{\pm}5.11$, and $2,024.34{\pm}134.18\;{\mu}g/g$, respectively. Under this optimal conditions, the contents of phytochemicals 1-3 in peanut pods of 3 Korea cultivars including 'Jakwang', 'Daekwang', and 'Palkwang' exhibited phytochemical 3 was the highest range of $1,338.01-5,162.93\;{\mu}g/g$, followed by phytochemical 1 ($590.13-1,382.10\;{\mu}g/g$), and phytochemical 2 ($25.12-186.85\;{\mu}g/g$), respectively. Moreover, 'Jakwang' exhibited the highest contents of phytochemical (1: $1,362.10{\pm}52.49$, 2: $186.85{\pm}17.69$, and 3: $5,162.93{\pm}148.64\;{\mu}g/g$, respectively), whereas the lowest contents was found in the 'Daekwang' (1: $590.13{\pm}22.23$, 2: $25.12{\pm}2.45$, and 3: $1,338.01{\pm}62.17\;{\mu}g/g$, respectively). These results suggest that the methanol extracts of peanut pods may possess health related benefits to humans owing to various known biological activities of phytochemicals 1-3.

• YAKHAK HOEJI
• /
• v.50 no.5
• /
• pp.313-321
• /
• 2006

There are three kinds of liquid petroleum marker which is extracted by the basic or acidic, and both developer. Korean marker, Unimark 1494 DB (marker) have been spectrophotometrically analysed by the determination of absorbance at 582 nm after base extraction by Unimark 1494 DB Developer C-5 (developer). Some blue dyes which have same reactive radical of marker and can be changed deep blue color in base developer extraction (BDE), may be increased absorbance at 582 nm, but dyes or markers which can be increased the absorbance, were not unclear. In this experiment, effects of three dyes or marker such as Orimax Green 151 (the mixture of CI Solvent Yellow 16 and CI Solvent Blue 70), quinizarin and Orimax Blue 2N (CI Solvent Blue 35), and two solvent such as topasol (P-250) and lubricant (P-8) on the absorbance were studied by HITACHI Recording Spectrophotometer U-3300. It shows that all of them increased absorbance at 582 nm after BDE. Absorbance at 582 nm can be showed 0.0544 by Orimax Green 151 at the concentration of 3.96 mg/l, quinizarin at the concentration of 1.38 mg/l, and Orimax Blue 2N at the concentration of 2.73 mg/l in the artificial petroleum (normal diesel oil: topasol: lubricant=2 : 4: 4), respectively. Absorbance, 0.0544 indicates that concentration of marker is 1.64 mg/l in the reference curves, respectively. And also these results can be showed that the artificial petroleum have about 10% cheep fuel such as kerosene which have marker (16.0 mg/l). Absorbance of P-250 was 0.01361-0.22842 depending upon the purchasing date, and that of P-8 was 0.05644. pH of developer was 14.83, and so this result indicates that Unimark 1494 DB is a base extractable petroleum marker, phenylazophenol (US Patent No. 5,252,106). In the BDE, the slight color of Orimax Blue 2N, Orimax Green 151 and quinizarin in artificial petroleum changed to deep bright blue color, respectively. These result indicate that the absorbance at 582 nm by BDE may be increased not only by azo, diazo, amine and ketone (anthraquinone, coumarin) dyes or markers, but also the contaminants of P-250 and P-8 which have same as reactive radical of dyes or markers.

• Analytical Science and Technology
• /
• v.11 no.5
• /
• pp.374-385
• /
• 1998

Phytoestrogens are biologically active compounds derived from plants foods. It had been suggested that phytoestrogens, by inhibiting aromatase in peripheral and/or cancer cells and lowering estrogen levels, may play a protective role as antipromotional compounds during growth of estrogen-dependent cancers. Therefore, simultaneous analysis of estrogens and phytoestrogens is necessary to elucidate the possible involvement of phytoestrogens in estrogen metabolism. In this view, we developed a simple and reproducible procedure to quantitatively determine estrogen and phytoestrogen metabolites. The proposed method consisted of solid phase extraction using preconditioned Serdolit AD-2 resin, enzyme hydrolysis with ${\beta}$-glucuronidase/arylsulfatase from Helix pomatia, liquid-liquid extraction and TMS-ether derivatization. And the final determination was carried out by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode (SIM). The precision and accuracy of this method was evaluated through within-a-day and day-to-day test. Recovery range and detection limit were 71.96~105.66%, 2~4 ng/mL, respectively. Using this method, 17 estrogen and 5 phytoestrogen compositions in urine of normal subjects were analyzed. It was found that amounts and relative distribution of urinary phytoestrigens and estrogens showed different pattern in male and female subjects.

• Journal of Environmental Science International
• /
• v.15 no.1
• /
• pp.85-94
• /
• 2006

The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

• Journal of Radiation Protection and Research
• /
• v.20 no.4
• /
• pp.275-283
• /
• 1995

PERALS(Photon Electron Rejecting Alpha Liquid Scintillation) spectrometry coupled with solvent extraction method has been set up for the analysis of $^{222}Rn\;and\;^{226}Ra$ in the groundwater. This analytical method offers low background, better energy resolution and lower quenching problem than the other techniques. By the analysis of NIST SRM 4966 $^{226}Ra$ standard, the analytical accuracy and precision were found to be 3% and 1%, respectively, and the relative standard deviation of the recovery of Rn extraction between pH2 and pH10 was 7%. Detection limits of $^{222}Rn$ and $^{226}Ra$ for 10 hours counting were counted to be $0.42 pCi/{\iota}\;and\;0.016 pCi/{\iota}$, respectively. For the test analysis of $^{222}Rn\;and\;^{226}Ra$ in the graundwater, hot spring water samples of 17 regions were analyzed. The concentration of $^{222}Rn$ were in the range of $90{\sim}5200pCi/{\iota}$ and average value was $1470pCi/{\iota}\;^{226}Ra$ concentration showed a peak value of $97.9pCi/{\iota}$ in a Kangwon region, but the average value was $1.14pCi/{\iota}$ except that region.

• Environmental Analysis Health and Toxicology
• /
• v.5 no.3_4
• /
• pp.19-28
• /
• 1990

Nitroarenes are ubiquitous environmental pollutants displaying potent mutagenicity in bacteria and carcinogenicity in mammal. In this study, the concentration of nitroarenes in coarse and fine particles and mutagenicity of POC$\_$N/ fraction was investigated in suspended particulates at the Shinchon and Bulkwang area of Seoul. The suspended particulates were collected bimonthly by a high volume cascade impactor air sampler from July 1987 to May 1988. Extractable organic matter was obtained by ultrasonic extraction on diethly ether/cyclohexane (8/2, v/v). Neutral fraction was obtained by liquid-liquid extraction. Polar neutral organic compounds (POC$\_$N/) was fractionated by thin-layer chromatography. Finally, the concentrations of nitroarenes in POC$\_$N/ fraction were measured and determined by capillary gas chromatography. Direct and indirect mutagenicity of POC$\_$N/ fraction were measured using Salmonella typhimurium TA 98. The result were as follows: 1) Major nitroarenes at the Shinchon area was 1-nitropyrene and at the Bulkwang area it was 2,7-dinitro-9-fluorenone during the year. 2) Average concentration of total nitroarenes measured was 67.26 ng/m$^3$in fine particles which was 1,3 folds higher that in coarse particle (52.30 ng/m$^3$). 3) Annual pattern of nitroarenes concentrations revealed that concentration during heating season (Feb., Jan., Mar.) was 2.2 folds higher than that in non heating season (May, Jul., Sep.). Concentration of each season has 157.68 ng/m$^3$and 80.39 ng/m$^3$. 4) The mutagenic activity of POC$\_$N/ fraction from fine particles was higher compared to that of coarse particles and was increased when metabolically activated, with 59 mixture. Mutagenicities, Metabolically activated, were significantly different between Shinchon and Bulkwang area, 322.8 rev/250 $\mu\textrm{g}$/plate and 286.8 rev/250 $\mu\textrm{g}$/plate, respectively. 5) Annual pattern of mutagenicity of POC$\_$N/ fraction revealed that mutagenicity during the heating season was 1.7 folds higher at Shinchon area and 1.2 folds higher at Bulkwang than during the non heating season. The variable contents and levels of nitroarenes in suspended particulates may affect human health significantly. Further studies such as risk assessment should be conducted on the basis of these kind of studies.

• Analytical Science and Technology
• /
• v.18 no.3
• /
• pp.201-205
• /
• 2005

Tri-octyl amine (TOA) is used in solvent extraction process for radioactive waste. This compound may be degraded to di-octyl amine (DOA), mono-octyl amine (MOA) by radioactive materials. Amount of TOA, DOA and MOA in TOA must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for TOA, DOA and MOA are studied with Phenomenex LUNA-$C_{18}$ ($4.6mm{\times}25cm$) analytical column and $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) eluent by liquid chromatography. Optimum condition for these compounds is $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) = 85 : 15 ratio. TOA, DOA and MOA compounds is well separated within 20 minute. Dynamic range is $30{\sim}160{\mu}g/mL$ for TOA, $5{\sim}100{\mu}g/mL$ for DOA and $0.1{\sim}5{\mu}g/mL$ for MOA, respectively. The detection limit are $0.1{\mu}g/mL$ for TOA, $1{\mu}g/mL$ for DOA (in SCAN mode) and $0.1{\mu}g/mL$ for MOA (in SIM mode) in this system with $20{\mu}L$ sample loop.

• Analytical Science and Technology
• /
• v.23 no.2
• /
• pp.179-186
• /
• 2010

The oxidative metabolism of ibuprofen in healthy male urine collected at 3, 6, 9, 12 and 15 h after oral administration of ibuprofen was studied by GC/MS assay. To detect conjugated metabolites of ibuprofen, urine sample was acid-hydrolyzed with 6 M HCl at $100^{\circ}C$ for 30 min. To effectively extract ibuprofen and its metabolites, liquid-liquid extraction (LLE) was conducted at pH 3, 5, and 7, respectively. As a result, LLE at pH 3 was shown to be the best extraction condition. For the determination of trace amounts of ibuprofen and its metabolites in extract, trimethylsilylation (TMS) with BSTFA was applied and followed by GC/MS analysis. In this study, main 5 metabolites including parent drug were detected and these metabolites were assigned as three hydroxylated forms and one carboxylated form. Each metabolite was tentatively identified by both interpretation of mass spectrum and comparison with previously reported results. In addition, time profile of urinary excretion rate for parent drugs and metabolites was studied. Finally, the metabolic pathways of ibuprofen were suggested on the basis of the structural elucidation of its metabolites and excretion profiles.

• Korean Journal of Food Science and Technology
• /
• v.49 no.5
• /
• pp.544-549
• /
• 2017

The spent coffee grounds (SCG) are considered valuable by-products because they contain various bioactive compounds. The SCG extraction (SCGE) was irradiated at doses ranging between 30 and 50 kGy. The deep dark-brown color of SCGE was changed to a bright yellow color by gamma irradiation. The content of the bioactive compounds of gamma-irradiated SCGE was analyzed by high-performance liquid chromatography. Interestingly, the content of quinic acid was increased by gamma irradiation, whereas other compounds were decreased. Although the contents of bioactive compounds were changed by gamma irradiation, the biological activities (radical scavenging activity and whitening effects) of SCGE were unaffected. Our findings suggest that gamma irradiation can effectively improve the color values of SCGE without the loss of biological activities. Consequently, gamma irradiation can be a useful tool for improving the utilization of SCGE in the cosmetic industry.