• Food Science and Preservation
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• v.22 no.4
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• pp.559-566
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• 2015

The aim of this study was to develop an analytical method for determination of T-2 toxin and HT-2 toxin level in cereals and to survey their levels using LC-MS/MS. The T-2 and HT-2 toxins were simultaneously analyzed by electrospray ionization with a positive ion mode and multiple reaction monitoring (MRM) after filteration and immuno-affinity column clean-up. A matrix-matched standard calibration used for quantification and recoveries of T-2 and HT-3 toxins were in the range of $100.6{\pm}7.2%$ and $96.8{\pm}9.4%$, respectively. Limits of detection and quantification of T-2 and HT-2 toxins were estimated to be 0.5 and $1.5{\mu}g/kg$, respectively. Each repeatability (RSRr) of T-2 and HT-2 toxins was determined to be 0.9~6.0%, and 4.9~6.1%, respectively. Total 115 samples cereals were collected from 9 types of cereals for analysis. The positive percentages of T-2 and HT-2 toxins obtained from collected samples were found to be 72% and 80%, respectively. The contamination level of T-2 toxin and HT-2 toxin in cereals were $37.1{\mu}g/kg$, and $5.4{\mu}g/kg$, respectively. Therefore, this study suggests that the developed method could be an useful analytical method to determine the T-2 and HT-2 toxin level in cereals and the present data could be used as a reference to estimate the risk assessment.

• Analytical Science and Technology
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• v.18 no.6
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• pp.453-459
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• 2005

Phenol compounds in water were simultaneously analyzed by extractive derivatization. Aqueous solution was controlled to pH 13 with sodium hydroxide, and then $500{\mu}L$ of benzoyl chloride was added to the solution. The solution was shaken for 15 minutes and extracted with diethyl ether and then analyzed using GC/MS-SIM. The calibration curves of phenolic compounds in the range of 0.05 to $5.0{\mu}g/mL$ showed a good linearity having the correlation coefficient of $r^2=0.9915$ and standard deviation of ${\leq}8.5%$, respectively. The recoveries by this method ware 58.4-114.0%.

• Analytical Science and Technology
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• v.23 no.4
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• pp.405-413
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• 2010

A new method for the simultaneous determination of six glucocorticoids (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, and flumethasone) in meats (bovine muscle, bovine liver) were established. Samples were effectively extracted using C18 cartridge with ethylacetate. Chromatographic separation was achieved using C18 column and negative electrospray ionization mass spectrometry was performed in the Multiple Reaction Monitoring mode for the effective quantitation and qualification of glucocorticoids. Acetonitrile and water (0.1% formic acid) were used as mobile phase and additive for effective electrospray ionization, and gave good chromatographic separation and mass spectrometric sensitivity. The limit of detection (LODs) and the limit of quantitation (LOQs) in spiked blank samples depending on types of matrix and pharmaceuticals were ranged from 0.2 to $1.0\;{\mu}g$/kg and 0.8 to $3.4\;{\mu}g$/kg, respectively. And the recoveries were between 89.5 to 119.6%. The established method showed good recoveries, accuracies, precisions and fast sample preparation and it will be applied to assay of glucocorticoids residues in meat.

• Environmental Analysis Health and Toxicology
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• v.26
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• pp.12.1-12.7
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• 2011

Objectives: Perchlorate is an emerging contaminant that is found everywhere, including various foods. Perchlorate is known to disturb the production of thyroid hormones and leads to mental disorders in fetuses and infants, as well as metabolic problems in adults. In this study, we attempted to establish an LC-MS/MS method for measuring perchlorate in dairy products and used this developed method to investigate perchlorate levels in Korean milk and yogurt samples. Methods: The developed method of perchlorate analysis requires a shaker and 1% acetic acid/acetonitrile as the extracting solvent. Briefly, the samples were extracted and then centrifuged (4000 rpm, 1hour), and the supernatant was then passed through a $Envi^{TM}$ Carb SPE cartridge that had been prewashed sequentially with 6 mL of acetonitrile and 6 mL of 1% acetic acid in water. The final volume of the sample extract was adjusted to 40 mL with reagent water and the final sample was filtered through a 0.20-${\mu}m$ pore size PTFE (Polytetrafluoroethylene) syringe filter prior to LC-MS/MS. Results: The average levels of perchlorate in milk and yogurt samples were $5.63{\pm}3.49\;{\mu}g/L$ and $3.65{\pm}2.42\;{\mu}g/L$, respectively. The perchlorate levels observed in milk samples in this study were similar to those reported from China, Japan, and the United States. Conclusions: The exposure of Koreans to perchlorate through the consumption of dairy products was calculated based on the results of this study. For all age groups, the calculated exposure to perchlorate was below the reference of dose (0.7 ${\mu}g/kg$-day) proposed by the National Academy of Science, USA, but the perchlorate exposure of children was higher than that of adults. Therefore, further investigation of perchlorate in other food samples is needed to enable a more exact assessment of exposure of children to perchlorate.

• Analytical Science and Technology
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• v.21 no.6
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• pp.495-501
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• 2008

Agilent 5973 GC-MS instrument was modified so that the capillary direct interface was removed and that a silicone membrane was installed between GC and MS. Feasibility study of the membrane interface GC-MS has been carried out. Vacuum of the mass spectrometer was not affected by the carrier gas flow rate up to $4.7m{\ell}/min$. As the carrier flow rate was increased, peak tailing was reduced and chromatogram peaks appeared earlier. Chromatogram peaks showed better separation and higher sensitivity as the membrane thickness was reduced from $127{\mu}m$ to $75{\mu}m$, and also as the interface temperature was increased. However, the membrane interface GC-MS had drawbacks such as background ions at 73 and 147 m/z and poor peak separation due to peak tailing.

• Analytical Science and Technology
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• v.16 no.6
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• pp.488-498
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• 2003

By LC/MS/MS, the analytical method of sildenafil and its analogues (homosildenafil, vardenafil and tadalafil) used as used medical treatment of impotence was established. electrosprary ionization (ESI) and atmospheric pressure chemical ionization (APCI) as a ionization method were applied. Several parameter were varied and the sensitivity and reproducibility were compared. In LC/ESI-MS method, capillary voltage, cone voltage, extractor, entrance and RF lens to create appropriate productr ions for multiple reaction monitoring (MRM) were variable parameter, but the formation of the other product ions except the precursor ion could not detect. And the value of entrance, collision energy, exit, corona voltage, cone voltage, extractor, RF lens, cone gas, and desolvation gas in APCI mode were varied, only the creation pattern of fragment ions by the change of RF lens value were detected, and the limit of detection was decreased due to the increase of S/N. Ten millimole ammonium formate (pH 4.8):acetonitrile=70:30 by isocratic elution in HPLC system was shown the maximum sensitivity in MS, the detection limit of sildenafil, homosildenafil, vardenafil and tadalafil obtained by ESI-MRM were 0.10, 0.025, 0.025, and $0.25{\mu}g/mL$ at S/N>5, respectively.

• Journal of Food Hygiene and Safety
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• v.20 no.4
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• pp.191-198
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• 2005

The purpose of this study was to determine the level of acrylamide in various processed foods, some of which were chosen because they were known to contain an excessive amount of acrylamide. A total of 190 food products based on steamed rice, cereals, and potato chips were purchased from retail markets and analyzed with the LC-MS/MS method. Acrylamide was found to be widely distributed in all of the foods. The fried Potato chips contained the highest levels of acrylamide, at $470-3,572{\mu}g/kg$; these were lowered to $38-633{\mu}g/kg$ by vacuum frying. The median concentration of acrylamide was higher in snacks containing potato ($448{\mu}g/kg$) than in those with no potato ($133{\mu}g/kg$). The concentrations of acrylamide were 2-96 $\mu$g/kg in Korean staple foods, $48-61{\mu}g/kg$ in bone-extract soups, and $0-57{\mu}g/kg$ in Bulgogi sauce. These results suggest that the components of processed ffods and the processing methods are important determinants of acrylamide formation.

• Analytical Science and Technology
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• v.16 no.6
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• pp.483-487
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• 2003

Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.

• The Journal of Korean Academy of Prosthodontics
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• v.50 no.4
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• pp.285-291
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• 2012

Purpose: This study was conducted to identify the surface characteristics of titanium discs coated with MS275/PLGA by electrospray and which is effective to mesenchymal stem cell proliferation. Materials and methods: We used anodized surface coated with PLGA as a control group and anodized surface coated with MS275 $0.5{\mu}M$, $1{\mu}M$, $1.5{\mu}M$ as test groups. To examine that the coating particles are nanometer sized, FE-SEM was used and AFM was utilized to determine the difference of coating surface roughness. We checked the mesenchymal stem cell proliferation by using MTT assay on $1^{st}$, $4^{th}$, $7^{th}$ days. Results: There was no significant difference between control groups and test groups in AFM results (P>.05). In MTT assay results, mesenchymal stem cell proliferation was increased with time, at $7^{th}$ day, cell viability on discs coated with $1.5{\mu}M$ MS275 was significantly higher than control group (P<.05). As SEM showed, the number of cells on all discs was increased and the morphology of cell attachment was also wider and closer with time. Conclusion: Titanium surface coated with MS275/PLGA showed significantly higher cell proliferation and the more density of MS275 was dispersed on titanium discs, the faster cells grew.

• ETRI Journal
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• v.32 no.5
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• pp.665-675
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• 2010

Recent research on mobile Internet protocol television and digital right management (DRM) interconnections has focused on multimedia technologies designed to enhance content scalability and adaptive content distribution. However, due to the architectural and scalable limitations, recent systems are not flexible and securable with respect to their adaptive content distribution and protective policy management. Therefore, we propose a content protective multi-agent platform that provides secure multimedia services, correlation management, pattern-based management, and multi-source multi-use (MsMu)-based services. Our architecture, supported by DRM, lets us create a rich set of MsMu-based content protection and seamless multimedia services through the extension of one source multi-use (OsMu)-based content services. We have verified our platform, which provides scalable and securable services with a 17% lower service response time by using a testbed.