• Food Science and Preservation
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• v.21 no.3
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• pp.381-387
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• 2014

Food irradiation is one of the successful modern techniques used to preserve food. However, it needs very careful control. Detection of irradiated food is of prime importance to facilitate global trade and consumer assurance, choice, and protection. This study was performed to evaluate the radiation-induced hydrocarbon content of dried squid and octopus by e-beam irradiation. The samples were collected from supermarkets all over South Korea and irradiated with an e-beam at 0, 1, 3, 5, 7, and 10 kGy doses. Lipids were extracted with soxhelt, and the hydrocarbons induced with irradiation were separated via solid phase extraction (SPE) and identified via gas chromatography mass spectrometry (GC/MS). The major induced hydrocarbons in the irradiated dried squid and octopus were 1-tetradecene and pentadecane derived from palmitic acid and 1-hexadecene and heptadecane from stearic acid. The concentration of hydrocarbons differed from the composition of the fatty acid at the same radiation and increased according to the level of the radiation dose. The hydrocarbons induced by e-beam irradiation, including 1-tetradecene, 1-hexadecene, and heptadecane, were confirmed to have been the irradiation marker compounds. Therefore, they can be used to distinguish the e-beam-irradiated dried squid and octopus from the non-irradiated ones.

• Journal of Environmental Health Sciences
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• v.29 no.2
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• pp.50-55
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• 2003

3,3-dichlorobenzidine is suspected to be cancinogenic in experimental animal and human. Several studies have investigated excretion of metabolites in urine, hemoglobin adduction and cancer incidence among workers occupationally exposed to 3,3'-dichlorobenzidine. In these researches, metabolites of 3,3'-dichlorobenzidine had a very important role, and were required as highly purity. The purpose of this study was synthesis and isolation of its metabolites from 3,3'-dichlorobenzidine. 3,3'-dichlorobenzidine was partially dissolved in benzene, ether, ethanol and methanol, and completely dissolved in 70% acetic acid on mixtures of citric acid containing less than 1% DCB, pyridine, a mixture of 0.5N NaOH and toluene(1:2), and phenol saturated with 20 mM TRIZA base. DCB, monoacetyl-DCB and diacetyl-DCB were measured by using gas chromatography/mass spectrometry(GC/MS). Detection for checking them was nitrogen phosphorous detection mode(NPD), and for identifying them was selected ion monitoring mode(SIM). The base peaks were 252 m/z in DCB, 252, and 294 m/z in monoacetyl-DCB, and 252, 294 and 336 m/z in diacetyl-DCB, respectively. Diacetyl-DCB was synthesized by titrating DCB solution of pyridine with sufficient acetyl chloride. Precipitation was diacetyl-DCB, which was purity of 98.7%. And its supernatant was composed of DCB, monoacetyl-DCB and diacetyl-DCB. By using acetic acid as controller of acetylation, monoacetyl-DCB was isolated from diacetyl-DCB . And residual pyridine was removed by using acetone. The purity of monoacetyl-DCB was 98.8%.

• The Korean Journal of Food And Nutrition
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• v.17 no.3
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• pp.260-265
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• 2004

Volatile components of pine needle(Pinus densiflora S.) were isolated by purge & trap headspace technique and analyzed by gas chromatography-mass spectrometry(GC-MS). And then volatile components were extracted for 2 hr and 20 hr at the two different temperature settings: room temperature and 60$^{\circ}C$. A total of 61 volatile components were identified by the four different conditions. These compounds are classified into six categories in terms of chemical functionality: 35 hydrocarbons, 16 alcohols, 4 carbonyls, 2 esters, 1 acid and 3 ethers. The major components were ${\alpha}$-pinene(1.5～15.7%), ${\beta}$-myrcene(13.2～15.6%), ${\beta}$-phellandrene(l2.0～16.0%) and cis-3-hexenol(4.0～18.3%). In the comparison of the four extraction conditions, longer extraction can be effective to extract components that have a high boiling point, but proved useless in obtaining low boiling point components. As a result of these experiments under the four different conditions, the 20 hr extraction at room temperature appeared to be the most optimized condition for the analysis of volatile compounds by using the purge & trap headspace technique.

• Journal of Ginseng Research
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• v.32 no.4
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• pp.305-310
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• 2008

The volatile constituents of the fresh roots of Panax ginseng C.A. Meyer have been investigated after treatment with artificial saliva and analysed by gas chromatography-mass spectrometry (GC-MS) using solid phase microextraction (SPME) fiber. Twenty peaks were detected in fresh ginseng, 5 of them were unknown peak, and mainly hydrocarbon components (${\alpha}$-pinene, ${\beta}$-pinene, myrcene, limonene, ${\beta}$-panasinsene, ${\beta}$-elemene, ${\beta}$-gurjunene, trans-caryophyllene, ${\alpha}$-gurjunene, ${\alpha}$-panasinsene, ${\alpha}$-neoclovene, trans-${\beta}$-farnasene, ${\alpha}$-humulene, ${\beta}$-neoclovene, ${\alpha}$-selinene, ${\beta}$-selinene, bicyclogermacrene) were detected. It's area percentage was increased about 10% in the fresh ginseng added artificial saliva during 40 minutes.

• Journal of the Korean Society of Food Science and Nutrition
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• v.31 no.6
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• pp.958-964
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• 2002

To select the irradiation-induced marker components from volatile flavor compounds in irradiated chicken, and complement the extraction problems of liquid continuous extraction (LLCE) method, the volatile compounds of irradiated (0,1,3,5 and 10 kGy) chicken were analyzed by Purge and Trap (P&T) and gas chromatography/mass spectrometry (GC/MS) methods. A total of 119 compounds were detected in irradiated chicken, and these compounds were composed mainly of 7 aldehydes,22 ketones,8 alcohols,30 esters,36 hydrocarbons,8 aromatic compounds and 8 miscellaneous compounds. Among these, only 21 compounds were detected in both LLCE and P&T methods, and the 98 other were detected in omly P&T method. Among volatile compounds detected in irradiated chicken, only 3 compounds such as hexene (r=0.96, p<0.01), propanol (r=0.93, p<0.05) and 1,3-bis(1,1-dimethylethyl) benzene (r=0.96, p<0.05) were newly selected as marker compounds in irradiated chicken by P&T method, which showed significant and high positive correlation coefficient in the change of relative concentration according to the increment of irradiation dosage.

• Analytical Science and Technology
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• v.12 no.3
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• pp.190-195
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• 1999

The metabolism of testosterone ($17{\beta}$-hydroxy-androst-4-en-3-one) was confirmed in horse after a single intramuscular administration of testosterone cypionate (750 mg). Solvent extracts of urine obtained with enzymatic hydrolysis and methanolysis were analyzed by GC/MS after oxime t-butyldimethylsilyl (oxime-TBDMS) derivatization. The structures of four urinary metabolite after testosterone administration in horse were determined based on EI mass spectra and $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol and $5{\alpha}$-androstane-$3{\beta}$-ol-17-one as major was confirmed with authentic standard. Also the concentrations of $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol, $5{\alpha}$-androstane-$3{\beta}$, $17{\beta}$-diol, dehydroepiandrosterone (DHEA), $5{\alpha}$-androstane-$3{\beta}$-ol-17-one and testosterone were determined in the urine of normal subjects and the urine after administration. The recovery and detection limit in the most drugs were 86.3~94.7% and 1~3 ppb, respectively. Correlation coefficients for calibration were in the range of 0.984~0.999. Excretion profile of testosterone presents the rapid and large increasement up to maximum values at days 5 after administration and the slow regression. The relative ratios of testosterone, its metabolites over DHEA were determined for indication of testosterone administration in horse doping.

• Food Science and Preservation
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• v.23 no.1
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• pp.63-73
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• 2016

The volatile flavor components of the fruit pulp and peel of orange (Citrus sinensis) and grapefruit (Citrus paradisi) were extracted by simultaneous distillation-extraction (SDE) using a solvent mixture of n-pentane and diethyl ether (1:1, v/v) and analyzed by gas chromatography-mass spectrometry (GC-MS). The total volatile flavor contents in the pulp and peel of orange were 120.55 and 4,510.81 mg/kg, respectively, while those in the pulp and peel of grapefruit were 195.60 and 4,223.68 mg/kg, respectively. The monoterpene limonene was identified as the major voltile flavor compound in both orange and grapefruit, exhibiting contents of 65.32 and 3,008.10 mg/kg in the pulp and peel of orange, respectively, and 105.00 and 1,870.24 mg/kg in the pulp and peel of grapefruit, respectively. Limonene, sabinene, ${\alpha}$-pinene, ${\beta}$-myrcene, linalool, (Z)-limonene oxide, and (E)-limonene oxide were the main volatile flavor components of both orange and grapefruit. The distinctive component of orange was valencene, while grapefruit contained (E)-caryophyllene and nootkatone. $\delta$-3-Carene, ${\alpha}$-terpinolene, borneol, citronellyl acetate, piperitone, and ${\beta}$-copaene were detected in orange but not in grapefruit. Conversely, grapefruit contained ${\beta}$-pinene, ${\alpha}$-terpinyl acetate, bicyclogermacrene, nootkatol, ${\beta}$-cubebene, and sesquisabinene, while orange did not. Phenylacetaldehyde, camphor, limona ketone and (Z)-caryophyllene were identified in the pulp of both fruits, while ${\alpha}$-thujene, citronellal, citronellol, ${\alpha}$-sinensal, ${\gamma}$-muurolene and germacrene D were detected in the peel of both fresh fruit samples.

• YAKHAK HOEJI
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• v.52 no.6
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• pp.419-425
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• 2008

A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

• Food Science and Preservation
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• v.23 no.7
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• pp.977-988
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• 2016

The volatile flavor compounds in five Jeju citrus fruit varieties (Cheonhyehyang, Hallabong, Jinjihyang, Hwanggeum hyang and Redhyang) were extracted by simultaneous distillation-extraction (SDE) using solvent mixture of n-pentane and diethyl ether (1:1, v/v) and analyzed by using gas chromatography-mass spectrometry (GC-MS). The number of aroma compounds were identified with : 104 (4,939.77 mg/kg) in Cheonhyehyang, 98 (3,286.38 mg/kg) in Hallabong, 105 (3,317.56 mg/kg) in Jinjihyang, 102 (4,293.39 mg/kg) in Hwanggeumhyang, and 108 (4,049.94 mg/kg) in Redhyang. The detected main volatile compounds were; limonene, sabinene, ${\beta}$-myrcene, ${\alpha}$-pinene, ${\beta}$-pinene, linalool, 4-terpineol, ${\alpha}$-terpineol, (E)-${\beta}$-ocimene and ${\gamma}$-terpinene. Among the identified volatiles compounds, ethyl-benzene, nonanol, 1-p-menthen-9-al, (E)-isocarveol, methyl salicylate, ${\alpha}$-terpinen-7-al, perilla alcohol, and ethyl-dodecanoate were detected in Cheonhyehyang. only Furthermore, ${\beta}$-chamigrene and ${\alpha}$-selinene were in Hallabong only; 3-hydroxybutanal, (E)-2-nonenal, isoborneol, octyl acetate, (E)-2-undecenal, ${\beta}$-ylangene and guaia-6,9-diene in Jinjihyang. ${\rho}$-Cymenene, ${\beta}$-thujone, selina-4,11-diene and (E,E)-2,6-farnesol in Hwanggeumhyang only; and ${\rho}$-cymen-8-ol, bornyl acetate, carvacrol, bicycloelemene, ${\alpha}$-cubebene and 7-epi-${\alpha}$-selinene in Redhyang only. This study confirmed the differences in composition and content of volatile aroma components in five varieties of Jeju citrus fruits.

• Microbiology and Biotechnology Letters
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• v.42 no.1
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• pp.11-17
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• 2014

Selenium is an essential trace element for mammals, but it is very toxic. Therefore, the control of selenium concentrations should be precisely and effectively monitored. Selenium is naturally obtained through foods and seleno-L-methionine (LSeMet) is a major form of selenium. It has been reported that L-SeMet is only converted into Se-adenosyl-L-SeMet. However, a recent study suggested that L-SeMet was directly metabolized into methylselenol ($CH_3SeH$) in mouse liver extract by the reaction of cystathionine ${\gamma}$-lyase (CGL). The canonical reaction of CGL was known to catalyze the cleavage of L-cystathionine to L-cysteine, ${\alpha}$-ketobutyrate and $NH_3$. In the present study, we found that L-SeMet could be directly converted to $CH_3SeH$ using purified homogenous human CGL instead of mouse liver cytosol. Authentic $CH_3SeH$ was prepared by reduction of dimethyldiselenide with sodium tetrahydroborate. The gaseous product of the enzymatic reaction with L-SeMet was analyzed by GC/MS spectrometry. The GC/MS data was identical to that of authentic dinitrophenyl selenoether. We also analyzed the kinetic parameters for the formation of $CH_3SeH$ from L-SeMet by human and mouse CGL. These results suggest that human CGL is a critical enzyme which is responsible for L-SeMet metabolism.