• Archives of Pharmacal Research
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• v.20 no.3
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• pp.247-252
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• 1997

Perfluorotolyl (PFT)-ether and perfluorotoly-trimethylsilyl (PFT-TMS) ether derivatives of oestrone, $17{\alpha}$- and $17{\beta}$oestradiol were prepared under phase transfer conditons. The former derivatives under negative ion chemical ionization conditions gave significant ions in the mass spectrometer but $17{\alpha}$- and $17{\beta}$ -oestradiol gave poor resolution. However, the PFT-TMS derivatives of 17.${\alpha}$- and$17{\beta}$-oestradiol showed good resolution. These derivatives were used for the analysis of oestrogens in bovine aqueous humour, vitreous humour and retina. The mean $({\pm}SEM)$ concentrations of oestrone in bovine aqueous humour (n=18), vitreous humour (n=18) and bovine retina (n=4) were $0.47{\pm}0.11$, $0.46{\pm}0.14$ and $1.10{\pm}0.24 ng.ml^{-1}$, respectively. $17{\alpha}$-Oestradiol was detected in 16 out of 18 samples of bovine aqueous humour and vitreous humour and the mean $({\pm}SEM)$ concentrations were $0.30{\pm}0.10$ and $0.08{\pm}0.02 ng.ml^{-1}$, respectively. The mean $({\pm}SEM)$ concentration of 17.betha.-oestradiol in aqueous humour (n=7) and vitreous homour (n=11) $0.83{\pm}0.26 ng ml^{-1}$ and $0.39{\pm}0.09 ng ml^-1$, respectively. In retina the concentrations of both steroids were below the detection limit.

• Analytical Science and Technology
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• v.13 no.4
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• pp.484-493
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• 2000

The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

• Journal of Food Hygiene and Safety
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• v.27 no.4
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• pp.473-478
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• 2012

The nutritional properties of the Kochujang were investigated with Fermented Extract of Hizikia fusiforme. No big differences in proximate compositions(moisture, Crude protein, Crude fat, and Crude ash, Carbohyrate) were observed between Two kinds of kochujangs tested in this study, general kochujang purchased from a market(GK), kochujang added with Fermented Extract of Hizikia fusiforme(FGK). However, FGK showed higher level of Total free amino acid(15,929.5 ng/mg), amino nitrogen(1715.88 mg%) and mineral contens than GK. the analysis of volatile compounds using GC/MS revealde than the fermentation dramatically removed off-flavors such as Acetaldehyde, Silane rimethyl(2-methylphenyl)-, 1H-Indole 2-phenyl-1-(trimethylsilyl) in Fermented Extract of Hizikia fusiforme(FGK).

• Journal of the Korean Magnetic Resonance Society
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• v.17 no.2
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• pp.98-104
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• 2013

The ERETIC (Electronic REference To access In vivo Concentrations)2 method is a new qNMR experimental technique to measure analytes based on the signal of the reference compound without additional hardware equipment. In this study, ERETIC2 method was validated, and we sought to identify whether it would be possible to apply this method to a specific compound analysis of metabolites in plant. The $90^{\circ}$ pulse value (P1) and spin-lattice relaxation time ($T_1$) of each compound were measured for ERETIC2. The $9^1H$ of 3-(trimethylsilyl) propionic-2,2,3,3-$d_4$ acid (TSP) was used as a reference peak for ERETIC 2, and then, a suitable solvent and pulse sequence for each compound were selected. Under the NOESY-presat sequence, the relative accuracy error for quantitative analyses of primary metabolites was within the range of 5%, with the exception of glucose, which showed ${\geq}$ 55% error due to saturation. It showed excellent results for the quantification of glucose by using a $30^{\circ}$ pulse sequence, which did not suppress the water peak. In addition, the quantitative accuracy for secondary metabolites was extremely accurate, with an error ${\leq}$5% when considering the purity of the standard sample. The ERETIC2 method showed outstanding linearity, precision, and accuracy.

• YAKHAK HOEJI
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• v.52 no.3
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• pp.172-175
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• 2008

Stable isotope ratio of carbon and nitrogen ($\delta^{13}C$ & $\delta^{15}N$), and $\Delta^{9}$-tetrahydrocannabinol (THC) contents were measured on 37 Korean cannabis and 10 commercial grade marijuana seized in Korea. Factors influencing on the measured values and their variations were investigated. $\delta^{13}C$ value of cannabis is specified mainly by water availability. Korean cannabis showed relatively low $\delta^{13}C$ values ranging -33.29$\sim$-27.01% (mean=-31.01%), which reflect geographic conditions of Korea where is rainy, especially during summer. $\delta^{15}N$ values, which reflect individual planting conditions, were relatively high up to -0.5$\sim$18.0% (mean=6.44%). It reflects characteristics of Korean cannabis growing wild in forest or cultivated in fertile soil. Tetrahydrocannabinol is the major hallucinogenic compound of cannabis. Ethanol extracts of cannabis leaves were derivatized by N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), and the derivatives were analyzed by GC-MS in selected ion monitoring (SIM) mode. THC contents of Korean cannabis ranged 0.11$\sim$4.34% (mean=1.47%), which were relatively low compared with commercial grade marijuana.

• Analytical Science and Technology
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• v.34 no.2
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• pp.68-77
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• 2021

Cannabis is one of the most abused drugs in Korea. The main psychoactive component in cannabis, Δ9-tetrahydrocannabinol, is metabolized to 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) and THCCOOH-glucuronide (THCCOOH-glu) in the human liver, whereby the amount of THCCOOH-glu found in urine is twice as high as that of THCCOOH. The analytical process adapted by the majority of urine drug-testing programs involves a two-step method consisting of an initial immunoassay-based screening test followed by a confirmatory test if the screening test result is positive. In this study, a qualitative gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the detection of THCCOOH in human urine, where THCCOOH-glu was converted into THCCOOH by alkaline hydrolysis. For purification of the urine extract prior to instrumental analysis, high-speed centrifugation was used to minimize interference. In addition, an injection-port derivatization method using ethyl acetate and N,O-bis(trimethylsilyl)-trifluoroacetamide containing 1 % trimethylchlorosilane was employed to reduce the time required for derivatization, and an aliquot of the final solution was injected into the GC-MS. The method was validated by measuring the selectivity, limit of detection (LOD), and repeatability. The sensitivity, specificity, precision, accuracy, Kappa, F-measure, false positive, and false negative rate were determined by comparing the GC-MS results with those obtained using the immunoassay. The LOD was determined to be 0.32 ng/mL, while the repeatability was within 9.1 % for THCCOOH. Furthermore, a comparison study was carried out, whereby the screening immunoassay exhibited a sensitivity of 86.4 % and a specificity of 100 % compared to GC-MS. The applicability of the developed method was examined by analyzing spiked urine and forensic urine samples obtained from suspected cannabis abusers (n = 221).

• Membrane Journal
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• v.28 no.2
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• pp.105-112
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• 2018

In this study, PTMSP-GO composite membranes were prepared by the addition of GO (graphene oxide) into PTMSP [poly (1-trimethylsilyl-1-propyne)] having high gas permeability, to study of gaseous membrane using GO. Gas permeation properties for $N_2$, $CH_4$, $CO_2$ were investigated by increasing the amount of GO in the PTMSP. PTMSP-GO composite membranes had higher gas permeability in the order of $N_2$ < $CH_4$ < $CO_2$. The gas permeation tendency of $N_2$, $CH_4$, and $CO_2$ increased as the content of GO increased from 0 to 10 wt%, but the gas permeability decreased as increased from 10 to 30 wt%. In the range of low GO contents, the gas permeability decreased due to the decrease of diffusivity because GO acts as a barrier in the composite membrane, and the gas permeability increased due to the void at the interface above the content range. And $CO_2$ has an affinity with -COOH of GO, the selectivity ($CO_2/N_2$) and the selectivity ($CO_2/CH_4$) gradually increase with increasing GO content. And the selectivity($CO_2/N_2$) showed the highest selectivity at 10.6 for PTMSP-GO 10 wt% and the selectivity ($CO_2/CH_4$) showed the highest selectivity at 3.4 for PTMSP-GO 20 wt%. However, above a certain amount of GO, selectivity ($CO_2/N_2$) and selectivity ($CO_2/CH_4$) decreased because the coagulation phenomenon between GO was increased and the solubility effect of $CO_2$ decreased. The PTMSP-GO 20 wt% composite membrane exhibited enhanced gas permeation characteristics with increased $CO_2$ permeability and selectivity ($CO_2/CH_4$) over PTMSP membrane.

• Korean Journal of Food Science and Technology
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• v.47 no.1
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• pp.27-36
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• 2015

The improved analytical method with gas chromatography (GC) and GC-mass spectrometry was established to identify and quantify disaccharides and trisacchrides in honey. In this method, the analysis of trimethylsilyl (TMS), TMS-oxime and TMS-methoxime sugars takes into account the determination of a single peak of complete separation on the chromatogram. The number of possible peaks for the qualitative and quantitative determination of TMS, TMS-oxime, and TMS-methoxime sugars was 17, 22, and 25, respectively. This new analytical method allowed for the determination of diand trisaccharides in honey by TMS-oxime and TMS-methoxime derivatives. This study suggested that the improved method is more suitable and precise than the other analytical methods for the simultaneous determination of sugars in honey.

• Journal of the Korean Chemical Society
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• v.42 no.3
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• pp.266-276
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• 1998

Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

• 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.