• Journal of the Society of Cosmetic Scientists of Korea
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• v.22 no.2
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• pp.153-160
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• 1996

A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

• YAKHAK HOEJI
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• v.19 no.4
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• pp.240-245
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• 1975

The quantitative analysis of ethambutol.2HCl as well as commercial ehambutol preparations was undertaken by gas-liquid chromatography by finding optimum conditions, such as the use of internal standard, stability of an ethambutol-2HCl-caffeine standard solution, and the effect of column temperature, N, O-bis-(trimethylsily) acetamide [B.S.A.] concentrations and other substances present in the preparations. Under the chromatiographic conditions, an ethambutol-2HCl. caffeine standard, 9 min, 30sec. The relative molar response of ethambutol.2HCl and caffeine studied was 2.08. Ethambutol.2HCl could be quantitated up to 1$\times$10$^{-8}$ moles. the possible decomposition of B.S.A. due to the moisture when tested and the incoplete reaction for silylation could be minimized.

• Bulletin of the Korean Chemical Society
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• v.26 no.6
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• pp.871-877
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• 2005

Recent progress in the filed of transition-metal mediated C-H bond activation has had a great influence on organic synthesis. Among such transition-metal catalyzed reactions, ortho-functionalization via the chelationassisted strategy has been paid great attentions as one of the powerful methodologies for converting aromatic compounds into ones that are more functionalized at the exclusively ortho-position. In this context, various transition metal-catalyzed ortho-functionalizations such as alkylation, alkenylation, silylation and carbonylation are described briefly and their prospects are suggested.

• Bulletin of the Korean Chemical Society
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• v.28 no.11
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• pp.1902-1909
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• 2007

This account reports an overview of our findings in homogeneous Pd-catalyzed reactions. Herein we describe the new design in reactions of Group 14 element compounds and in homogeneous nanosize Pd catalysts. In the early stages of our study, we developed Pd-catalyzed transformations of allylic esters with disilanes, silylcyanides and acylsilanes to the corresponding silylation, cyanation and acylation products, respectively. We also developed a Pd-catalyzed three component coupling reaction of Group 14 element compounds involving 1,3-diene and acid chlorides to form β,γ-unsaturated ketone as a single product. Recently, we focus our attention on modifying the catalytic environment by nanosize Pd in order to improve the performance of Pd catalysts. These nanosystems realize efficient catalytic environment with remarkable enhancement in catalytic activity and unprecedented selectivity.

• Journal of the Korean Applied Science and Technology
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• v.34 no.2
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• pp.260-270
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• 2017

Zirconia has white color and physical, chemical stability, also using in high temperature materials and various industrial structural ceramics such as heat insulating materials and refractories due to their low thermal conductivity, excellent strength, toughness, and corrosion resistance. If hydrophobically modified zirconia is introduced into a hydrophobic acrylate coating solution, the hardness, chemical, electrical, and optical properties will be improved due to the better dispersibility of inorganic particle in organic coating media. Thus, we introduced $-CH_3$ group through silylation reaction using either trimethylchlorosilane(TMCS) or hexamethyldisilazane(HMDZ) on zirconia surface. The $Si-CH_3$ peaks derived from TMCS and HMDZ on hydrophobically modified zirconia surface was confirmed by FT-IR ATR spectroscopy, and introduction of silicon was confirmed by FE-SEM/EDS and ICP-AES. In addition, the sedimentation rate result in acrylate monomer of the modified zirconia showed the improved dispersibility. Comparison of the sizes of a pristine and the modified zirconia particles, which were clearly measured not by the normal microscope but by particle size analysis, provided a pulverizing was occurred by physical force during the silylation process. From the BET analysis data, the specific surface area of zirconia was approximately $18m^2/g$ and did not significantly change during modification process.

• Journal of Food Hygiene and Safety
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• v.21 no.3
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• pp.153-158
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• 2006

The contamination levels of 3-MCPD(3-Monochloropropane-1,2-diol) and 1,3-DCP(1,3-Dichloro-2-Propanol) in soy sauce, sauces was monitored. 105 samples were collected from June 2005 to August 2005 in Gyeonggi-do. 3-MCPD and 1,3-DCP were analyzed by GCMSD. As results, the detection range of 3-MCPD concentration was between 0.02 mg/kg and 0.27 mg/kg in soy sauce. However any samples were not detected with 1,3-DCP. The contaminated rates of 3-MCPD in soy sauce was 17.1%. Soy sauce is the representative vegetable protein hydrolyzed food. The reliable analytical method f3r the toxic 3-MCPD and 1,3-DCP in Soy sauce has been studied. The derivatization studies of 3-MCPD and 1,3-DCP were performed mainly as Silylation with BSA(N,O-Bis(trimethylsilyl)-acetamide). The retention times of derivative, BSA-MCPD, BSA-DCP were 11.30 and 10.12 minutes.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.9 no.1
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• pp.23-40
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• 1999

The analysis of thiodiglycolic acid in urine has been used as an index of biological exposure to vinyl chloride. Unfortunately thiodiglycolic acid has a strong hydrophilic character, because it has two carboxylic groups, so that it can only be extracted with organic solvent with a great difficulty. Underivatized thiodiglycolic acid tends to tail because of non-specific interaction with the inert support. Therefore, esterification is the obvious first choice for derivatization of thiodiglycolic acid, particularly for gas chromatography. In this study, the focus of interest is to compare two method of esterifications (methylation and silylation). Methylation is to make the methyl ester of thiodiglycolic acid by reaction with diazomethane. Silylation is to make the trimethylsilyl ester of thiodiglycolic acid by reaction with N-trimethylsily-ldiethylamine. The results and conclusions are as the following: 1. The detection limit (sensitivity) of methylated thiodiglycolic acid was $5.00{\mu}g/m{\ell}$ and silylated thiodiglycolic acid was $3.07{\mu}g/m{\ell}$ by gas chromatography with flame ionization detector. 2. The optimal liquid-liquid extraction of thiodiglycolic acid was as following: To each of the tubes, $15m{\ell}$ of urine, concentrated sulfuric acid (pH 1 - 2) and 5 gsodium sulfate were added. The samples was extracted three times with $5m{\ell}$ ethylacetate each time. 3. The methylated thiodiglycolic acid was more stable than silylated thiodiglycolic acid in extractional solvent which contained humidity. 4. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.07324 in methylated thiodiglycolic acid with external standard calibration, and 0.07033 in methylated thiodiglycolic acid with internal standard calibration. 5. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.10914 in silylated thiodiglycolic acid with external standard calibration, and 0.13602 in silylated thiodiglycolic acid with internal standard calibration. From the above results, the analysis of methylated thiodiglycolic acid was more sensitive (limit of detection) than silylated thiodiglycolic acid by gas chromatography. However, the methylated thiodiglycolic acid was stable in the humidity and was separated sharply on chromatogram. Also, analysis of methylated thiodiglycolic acid was more precise (pooled coefficient of variation for 4 days) than silylated thiodiglycolic acid. In conclusion, it is established that the analysis of methylated thiodiglycolic acid is appropriate for biological monitoring of exposure to vinyl chloride.

• Korean Journal of Food Science and Technology
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• v.39 no.4
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• pp.360-365
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• 2007

The studies for the derivatization of 3-monochloropropane-1,2-diol (3-MCPD) were performed mainly as acylation with HFBI (heptafluorobutyrylimidazole), alkylation with PBA (phenylboric acid) and silylation with BSTFA (N,O-bis[trimethylsilyl]trifluoroacetamide). Also silylation with MTBSTFA(N-methyl-N-[tert.-butyldimethylsilyl] trifluoroacetamide) and acylation with MBTFA (N-Methyl-bis[trifluoro-acetamide]) were also considered. Except the TBDMS derivative of 3-MCPD, all the derivatives were detected well. The derivatives of 3-MCPD with HFBI, PBA and BSTFA showed below 10 ${\mu}g/kg$ which was sensitive enough to satisfy Korea maximum residue limit 0.3 mg/kg. Among the tested adsorbents, Extrelut20 and Florisil were evaluated as the proper adsorbents to eliminate the soy sauce matrix for 3-MCPD. Ethyl acetate was the most efficient eluent with good recovery rate. The desired surrogate compound and internal standard were 1,2-butanediol and 1,2-dibromo-3-chloropropane, respectively. The limit of detection for PB-MCPD and TMS-MCPD were 10.16 and 7.06 ${\mu}g/kg$ on GC/MSD, respectively. HFB-MCPD derivative showed the lowest detection limits 2.98 and 5.32 ${\mu}g/kg$ by GC/ECD and GC/MSD, respectively.

• Bulletin of the Korean Chemical Society
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• v.32 no.3
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• pp.809-814
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• 2011

A method based on the TMS derivatives and acidic hydrolysis was developed for the simultaneous determination of free and conjugated steroidal hormones in surface water. A silylation of five natural and two synthetic steroidal hormones was achieved with N-methyl-N-(trimethylsilyl) trifluoroacetamide/$NH_4I$ (1000:3) under catalysis of dithioerythritol for 60 min at $80^{\circ}C$. TMS derivatives of the steroid hormones containing multifunctional groups offer a single derivative product under this condition. The accuracy of the analytes was in the range of 87 to 110% at a concentration of 20 and 50 ng/L with relative standard deviations of less than 10%. The method detection limit was in the range of 0.01 to 0.02 ng/L for surface water. Natural steroidal hormones were detected in a concentration range of 0 to 1.03 ng/L in free form and 0 to 14.6 ng/L in conjugated form, respectively. We found that most of the natural hormonal steroids exist in conjugate forms (43 to 100%) in river water.

• Journal of the Korean Chemical Society
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• v.52 no.3
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• pp.239-248
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• 2008

study of the solid phase extraction (SPE) technique using activated carbon fiber (ACF) as a sorbent was carried out on the schedule chemicals in water. 14 different schedule chemicals, which are the hydrolysis products and simulants of chemical agents such as alkylphosphonate, thiodiglycol etc. were selected for the study. Pyridine was used as a promoter to increase the derivatization efficiency, especially to improve silylation of 3-quinuclidinol. To improve the recovery efficiency of amines in the water solution, 1 mL of 5% Et3N/MeOH was introduced into SPE-ACF before the water sample loading. Throughout this study, the optimum condition was established to detect rapidly above chemicals in water.