• Korean Journal of Food Science and Technology
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• v.31 no.6
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• pp.1495-1502
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• 1999

Gamma-irradiated beef and chicken at the dose levels of 0.5 to 10 kGy were subjected to the detection of radiation-induced 2-alkylcyclobutanones whether irradiated or not. Radiation-induced 2-alkylcyclobutanones were extracted from beef and chicken fats, separated by florisil column chromatography and identified with GC/MS method by selected ion monitoring(SIM). When beef and chicken were irradiated, 2-dodecylcyclobutanone, 2-tetradecylcyclobutanone and 2-(5'-tetradecenyl)cyclobutanone were formed from palmitic, stearic and oleic acids. Concentrations of 2-alkylcyclobutanones were linearly increased with the dose levels of irradiation and depended upon the composition of fatty acids in beef and chicken. Radiation-induced 2-alkylcyclobutanones in irradiated beef and chicken were remarkably detected at 1 kGy and over, while these compounds were not detected in non-irradiated samples. The concentrations of radiationinduced 2-alkylcyclobutanones were relatively constant during 6 months.

• Korean Journal of Food Science and Technology
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• v.43 no.5
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• pp.544-552
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• 2011

The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.

• Korean Chemical Engineering Research
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• v.48 no.2
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• pp.244-252
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• 2010

The objective of this study is to assess feasibility of simultaneous analysis for trace multi-components odorous and volatile organic compounds using a Triple-bed adsorbent tube with a thermal desorber and GC-MS. Triple-bed adsorbent tube is 3 bed packed Tenax-TA with small amount of Carbopack B and Carbosieve SIII in order of adsorption strength in a tube. The operating conditions of GC-MS was possibly able to and effectively detect high volatile and low molecular weight compounds at the mass range of 20~350 m/z using a below impurity 1ppm of Helium carrier gas, of which quantitatively analyzed by target ion extracts. According to the experiment, $C_1{\sim}C_5$ of 14 components; sulfur containing compounds(2), ketones(2), alcohols(4) and aldehydes(6) were simultaneously analyzed with recoveries of 99%, and good repeatability and linearity. High volatile and low molecular weight compounds such as methyl alcohol and acetaldehyde can be safely quantified with high recovery at a condition of 50mL/min of flow rate, below 2L of adsorption volume, and 45% of relative humidity. Target ion extract can also simultaneously quantify multicomponents with odorous and volatile organic compounds in an occasion of piled up two peaks.

• Analytical Science and Technology
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• v.22 no.5
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• pp.407-414
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• 2009

A simultaneous determination method for cholesterol, lanosterol and desmosterol was developed using gas chromatography/mass spectrometry. Urine was enzymatically hydrolyzed with ${\beta}$-glucuronidase/arylsulfatase. Samples were prepared using extractions with a mixture of ethyl acetate-hexane (2:3, v/v), followed by derivatization with a mixture of MSTFA/TMSI/TMCS (100:2:5 v/v/v). All analyses were performed using GC/MS in selective ion monitoring mode. Good linearities ($r^2=0.998{\sim}0.999$) in calibration curve and a satisfactory recovery (80.0%~113%) were achieved. Accuracy and precision values within ${\pm}15%$ in the concentration range of 5 to 200 ng/mL were also observed for all compounds. The developed method was applied to pravastatin-treated (70 and 250 mg/kg/day for 7 days, oral) hyperlipidemia rats. Those sterols were significantly lower in drug-treated rats compared to the controls, which justifies the drug efficacy. Therefore, these results indicate that the developed method was successfully applied to examine statin drug efficacy with urine sample.

• Korean Journal of Food Science and Technology
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• v.31 no.2
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• pp.441-447
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• 1999

Changes in flavor characteristics of roasted coffee in 6 package models during storage were investigated by GC/MS analysis and sensory evaluation to establish the criteria of the shelf-life of the roasted coffee in three flavor quality-'fresh', 'satisfying' and 'minimally acceptable' levels. In direct headspace method of GC/MS, 47 volatile compounds were analyzed and the light volatile compounds were reduced sharply at initial stage of storage and faster in the package with air. The correlation between % retention of 2,3-butanedione and overall aroma of roasted coffee showed good linear-relation, of which correlation coefficient (R) were from 0.999 to 0.904 depending on package models, indicating that 2,3-butanedione would be an index chemical for evaluating the freshness of roasted coffee. In sensory evaluation of 6 package models during storage, roasted whole beans (RB) and roasted and ground (RG) coffee in air-package were preserved in 'fresh quality' for $0.5{\sim}1$ week, 'satisfying quality' for $2{\sim}3$ weeks and 'minimally acceptable quality' for 12 weeks, while roasted whole beans in valve-package and roasted and ground coffees in vacuum-package, nitrogen-package and oxygen absorbent-package were preserved in 'fresh quality' for $2{\sim}4$ weeks, 'satisfying quality' for $12{\sim}24$ weeks and 'minimally acceptable quality' for 52 weeks. The oxygen absorbent-package was slightly less effective than other three methods.

• YAKHAK HOEJI
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• v.52 no.2
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• pp.137-146
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• 2008

Even though driving under the influence of drug (DUID) is a worldwide problem, we, Korea has no regulation system yet except for alcohol, and there are little cases reported related to DUID. In order to investigate the type of abused drugs for drivers in Korea, we tried to analyze controlled and non-controlled drugs in alcohol-positive blood samples. 275 whole bloods, which were positive for alcohol on the roadside test, were collected from the police for two months ($Nov.{\sim}Dec.$ 2006). The analytical strategy was constituted of three steps: First, alcohol in blood samples were confirmed and quantified by gas chromatography. Second, controlled drugs were screened by $Evidence_{investigator}\;^{TM}$ (Randox, U.K.) as preliminary test. It was based on immunoassay by biochip array analyzer. Nine groups of drug abuse were screened: amphetamines, methamphetamines, cannabis, cocaine, opiates, barbiturates, methadone, benzodiazepines I (oxazepam) & II (lorazepam). Finally, confirmation of these drugs was performed by GC-MS. Blood samples were extracted by solid-phase extraction by $RapidTrace^{TM}$ (Zymark, U.S.A.). After trimethylsilyl (TMS) derivatization, eluates were analyzed to GC-MS. Total 49 drugs were investigated in this study including controlled drugs, antidepressants, 1st generation antihistamines, dextromethorphan, nalbuphine, ketamine, etc. For rapid detection, we developed the automated identification system. It was made up a new software, "DrugMan", modified Chemstation data analysis menu and newly developed macro modules. A series of peak selection, identification and reporting of the results were performed automatically by this system. Concentrations of alcohol in 275 blood samples were ranged from 0.011 to 0.249% (average, 0.119%). Among 149 blood samples, just six samples (4.0%) were showed positive results to the immunoassay: one methamphetamine and five benzodiazepines group I. By GC-MS confirmation, only benzodiazepines were detected and methamphetamine was not detected from immunoassay positive blood sample. Besides these drugs, 5 chlorpheniramines, dextromethorphan, diazepam, doxylamine, ibuprofen, lidocaine and topiramate were also detected in whole bloods by GC-MS. Conclusively, the frequency of drug abuse for Korean drivers was relatively low. There was none case which illegal drug was detected. However these results were limited to alcohol positive blood samples, so it is necessary to analyze more samples including alcohol negative blood.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.45 no.3
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• pp.217-224
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• 2019

Phthalates, endocrine disrupting chemicals, are similar in structure to sex hormones and mainly show reproductive toxicity and developmental toxicity. In this study, we analyzed 11 phthalates, including 3 kinds of phthalates prohibited in cosmetic use and 8 kinds of phthalates regulated in 'Common standards for children's products safety' and EU cosmetic regulation (EC No. 1223/2009). The phthalate analysis was optimized using GC-MS/MS. In analytical method validation, this method was satisfied in specificity, linearity, recovery rate, accuracy and MQL. Therefore, we used this method to analyze 82 products of Nail cosmetics & polish. Although six phthalates such as DBP, BBP, DEHP, DPP, DIBP and DIDP were detected at concentrations of $1.0{\sim}59.8{\mu}g/g$g, they were suitable to Korean cosmetic standards. DIBP and DBP were detected at concentration of $1.1{\sim}2.6{\mu}g/g$ in artificial nail, DBP and DEHP were $1.4{\sim}2.5{\mu}g/g$ in glue for nails, and DIBP, DBP, and DEHP were $2.5{\sim}33.3{\mu}g/g$ in nail stickers. Although substances such as DBP and DEHP in artificial nail, Glue for nails, and nail stickers were detected, they were suitable to 'Common safety standards for children's products. DIBP is not a regulated substance in Korea but showed the third highest detection rate following DBP (84.6%) and DEHP (63.4%). The concentration of phthalates detected in nail products is considered to be safe in current standards but continuous monitoring and research about non-regulated substances are also needed to be considered.

• Analytical Science and Technology
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• v.15 no.6
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• pp.489-495
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• 2002

In this study, we determined distribution status of organonitrogen pesticides such as trifluralin, atrazine, metribuzin, alachlor, malathion, nitrofen, permethrin, cypermethrin, fenvalerate, and parathion accumulated in the fresh water fishes and amphibians. We collected those samples at 31 sites from the basin of major rivers, and separated the muscular tissue as a final sample for analysis. In the pretreatment process, lipid was eliminated by using acetonitrile and n-hexane, and pesticides were reextracted with dichloromethane. The extract was dehydrated and concentrated, and then cleaned it up by passing the Florisil column, and pesticide content was finally determined by using a GC-MS system after introducing isotope labelled references. The accumulation level was observed in the range of $0.17{\sim}6.8{\mu}g/kg$ in amphibians and $0.26{\sim}16{\mu}g/kg$ in fishes including cypermethrin as $16{\mu}g/kg$.

• Analytical Science and Technology
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• v.11 no.5
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• pp.353-359
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• 1998

Danazol, one of the IOC banned substances, is a synthetic steroid which stimulates the synthesis of cellular protein with multiple and diverse biologic effects. To confirm the androgenic effects of danazol, levels of eight endogenous steroids and its major metabolite in human urine were simultaneously analyzed by selected ion monitoring (SIM) of GC/MS after oral administration. The recovery range of this method was 71.59%~93.56% and the RSD values of precision and accuracy test were 1.87%~10.48% and 1.32%~11.25%, respectively. The limits of detection of most of the drugs were $0.01{\sim}0.05{\mu}g/mL$ and calibration was carried out using urine spiked with each endogenous steroid and ethisterone standard at a concentration of 0.1, 0.5, 1.0, 10, 20 and $50{\mu}g/mL$ and with $10{\mu}g/mL$ of internal standard. Correlation coefficients varied between 0.963 and 0.991. The endogenous steroid profiling is one of valuatle tool for decteation of anabolic steroids.

• Korean Journal of Food Science and Technology
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• v.30 no.3
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• pp.615-623
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• 1998

The garlic juices were extracted and concentrated by heating at $90^{\circ}C$, by using a rotary vacuum evaporator at $45^{\circ}C$, or by freezing at $-50^{\circ}C$ until the volume was reduced to 70% of the original volume. The concentrated juices were kept at $4^{\circ}C\;or\;25^{\circ}C$ for 60 days and the changes of bacteria and color were monitored every 10 days. Flavors of the raw garlic juices, concentrated garlic juices, and garlic powder by hot-air drying were analyzed monthly using GC and GC/MS. The CFUs/mL of mesophilic and psychrotrophic bacteria in the garlic juice concentrated at $90^{\circ}C$ were lower about 1 to 2 log cycles than those of other concentrated juices. Hunter L, a, and b values in the raw garlic raw juice and the juice concentrated at $-50^{\circ}C$ significantly increased at the beginning of storage, in particular, when they were stored at $25^{\circ}C$. The garlic juice concentrated at $45^{\circ}C$ showed relatively low L value but the juice concentrated at $90^{\circ}C$ showed high a value. The main peaks in chromatograms of volatile components identified by GC/MS were 3,3'-thiobis-1-propene, di-2-propenyl disulfide, 3-(methylthio)-1-propene in the raw garlic juice and the concentrated juices, and the juices concentrated at $45^{\circ}C\;or\;-50^{\circ}C$ showed relatively high preservation of garlic flavor.