• Journal of the Korean Magnetic Resonance Society
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• v.19 no.2
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• pp.67-73
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• 2015

The microcystin is a cyclic heptapeptide from metabolites of cyanobacteria in the genera mycrocystis, anabaeba as a result of eutrophication. It has been known that microcystin-LR is a potent inhibitor of the catalytic subunits of protein phosphatase-1 (PP-1) as well as powerful tumor promoter. The active site of microcystin actually has two metal ions $Fe^{2+}/Zn^{2+}$ close to the nucleophilic portion of PP-1-microcystin complex. We report the isolation and purification of this microcystin-LR from cyanobacteria (blue-green algae) obtained from Daechung Dam in Chung-cheong Do, Korea. Microcystin-LR was extracted from solid-phase extraction (SPE) sample preparation using a CN cartridge. The cyanobacteria extract was purified to obtain microcystin-LR by HPLC method and identified by LC/MS. The detail structural studies that can elucidate the possible role of monovalent and divalent metal ions in PP-1-microcystin complexation were carried out by utilizing molecular dynamics. Conformational changes in metal binding for ligands were monitored by molecular dynamic computation and potential of mean force (PMF) using the method of the free energy perturbation. The microcystin-metal binding PMF simulation results exhibit that microcystin can have very stable binding free energy of -10.95 kcal/mol by adopting the $Mg^{2+}$ ion at broad geometrical distribution of $0.5{\sim}4.5{\AA}$, and show that the $K^+$ ion can form a stable metal complex rather than other monovalent alkali metal ions.

• YAKHAK HOEJI
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• v.54 no.4
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• pp.226-231
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• 2010

Oral fluid has become increasingly popular as an alternative specimen in the field of driving under the influence of drugs (DUID) and work place drug testing. In this study, an analytical method for the detection and quantification of ${\Delta}^9$-tetrahydrocannabinol (THC) and its metabolite, 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THC-COOH) in oral fluid by SPE and GC-MS was established and fully validated. The stability of THC and THC-COOH in oral fluid during storage was also determined by examining the THC and THC-COOH concentration changes depending on time and container materials. Oral fluid samples were kept over 21 days at room temperature, $-4^{\circ}C$ and $-20^{\circ}C$ in two different specimen collection tubes; glass and polypropylene tubes. Three replicates for each condition with different temperature and types of a container were analyzed at five different time points over 21 days. When oral fluid samples were stored in glass tubes, the loss of both THC and THC-COOH was less than 10% at all room temperature, $-4^{\circ}C$ and $-20^{\circ}C$. However, in polypropylene tubes, the loss of both THC and THC-COOH increased significantly over the study period. In particular, the concentration of THC decreased more rapidly than that of THC-COOH at room temperature and the maximal percentage of THC lost was 90.3% after 21 days. The result indicates that it would be necessary to collect oral fluid samples in glass containers and cool the samples until analysis in order to prevent the degradation of analytes.

• Proceedings of the Korean Geotechical Society Conference
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• 2000.11a
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• pp.705-712
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• 2000

The fluid generally flows through fractures in crystalline rocks where most of underground storage facilities are constructed because of their low hydraulic conductivities. The fractured rock is better to be conceptualized with a discrete fracture concept, rather continuum approach. In the aspect of fluid flow in underground, the simultaneous flow of groundwater and gas should be considered in the cases of generation and leakage of gas in nuclear waste disposal facilities, air sparging process and soil vapor extraction for eliminating contaminants in soil or rock pore, and pneumatic fracturing for the improvement of permeability of rock mass. For the purpose of appropriate analysis of groundwater-gas flow, this study presents an unsteady-state multi-phase FEM fracture network simulator. Numerical simulation has been also conducted to investigate the hydraulic head distribution and air tightness around Ulsan LPG storage cavern. The recorded hydraulic head at the observation well Y was -5 to -10 m. From the results obtained by the developed model, it shows that the discrete fracture model yielded hydraulic head of -10 m, whereas great discrepancy with the field data was observed in the case of equivalent continuum modeling. The air tightness of individual fractures around cavern was examined according to two different operating pressures and as a result, only several numbers of fractures neighboring the cavern did not satisfy the criteria of air tightness at 882 kPa of cavern pressure. In the meantime, when operating pressure is 710.5 kPa, the most areas did not satisfy air tightness criteria. Finally, in the case of gas leaking from cavern to the surrounding rocks, the resulted hydraulic head and flowing pattern was changed and, therefore, gas was leaked out from the cavern ceiling and groundwater was flowed into the cavern through the walls.

• Journal of the Korean Chemical Society
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• v.21 no.5
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• pp.372-378
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• 1977

The following new techniques have been developed: (A); To a 500ml of sample water, it was adjusted pH 10 with ammonia-anmonium citrate, added 10ml of 1${\%}$ sodium diethyldithiocarbamate and extracted three times with 10ml of CHCl3. The extract was shaken with 10ml of 0.05N $HCl-4{\times}10^{-4}M\;HgCl_2$. The aqueous solution was added 2ml of 2N KCl and washed two times with 10ml of pure $CHCl_3$, and then recorded square wave polarograms. (B); To a 500ml of sample water adjusted pH 10 with ammonia-ammonium citrate, it was added 2ml of 1${\%}$ 8-hydroxyquinoline and extracted three times with 10ml $CHCl_3$. The separated $CHCl_3$ phase was shaken with 10ml of 0.2 N HCl. The aqueous solution was recorded polarograms directly. These methods can be used for determination of the ppb order of metal in water with an error of ${\pm}10{\%}$. The method (B) can not be used for the determination of zinc on account of the free 8-hydroxyquinoline.

• Journal of Korean Society of Water and Wastewater
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• v.32 no.5
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• pp.389-398
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• 2018

A nationwide survey of 8 N-nitrosamines in finished water samples from drinking water treatment plants (DWTPs) in Korea was conducted. The samples were pre-treated by solid-phase extraction (SPE) and analyzed using a gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). According to the study results, four N-nitrosamines (NDMA, NDEA, NMOR, NDBA) were detected for three consecutive years, NMEA and NPYR were only found in samples collected in 2013. Two of these N-nitrosamines, N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA), have received attention and were the most commonly detected. The concentration of NDMA and NDEA in this study ranged from $0.002{\mu}g/L$ to $0.013{\mu}g/L$ and in $0.001{\mu}g/L$ to $0.008{\mu}g/L$, respectively. In comparison to studies performed in EPA(UCMR2), the concentrations of NDMA (from $0.002{\mu}g/L$ to $0.630{\mu}g/L$) and NDEA (from $0.005{\mu}g/L$ to $0.100{\mu}g/L$) observed in the this study were low.

• Journal of the Korean Society of Food Science and Nutrition
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• v.41 no.6
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• pp.870-874
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• 2012

The objective of this study was to determine the content of capsaicinoids in different commercial pepper powders and pepper-containing products in the Korean market. The two major capsaicinoids in the samples, capsaicin and dihydrocapsaicin, were analyzed using reversed-phase HPLC. The levels of capsaicin and dihydrocapsaicin in pepper powders and pepper-containing products ranged from 0.21 to 78.24 and 0.20 to 38.82 mg/100 g sample, respectively. Pepper powders contained generally higher amounts of capsaicin and dihydrocapsaicin than pepper- containing products. In addition, the analytical method validation parameters including accuracy, precision, and specificity were provided to ensure the validity of the extraction procedure for capsaicinoid analysis. Overall recovery from pepper powder and pepper paste was close to 100% (n=3). The results of validation parameters indicated that the present method was reliable and reproducible for the HPLC analyses of capsaicin and dihydrocapsaicin in commercial pepper products.

• Natural Product Sciences
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• v.26 no.1
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• pp.64-70
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• 2020

Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.48 no.3
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• pp.301-307
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• 2015

Phlorotannins and marine algal polyphenols, including dieckol, 6,6-bieckol, phloroglucinol, phlorofucofuroeckol-A, and eckol, were isolated from brown seaweeds. These compounds have beneficial bioactivities, and Ecklonia cava has become widely used for the extraction and isolation of phlorotannins. Eckol, in particular, has been to shown to have antioxidant, anti-inflammatory, anticoagulatory, and photoprotective properties. However, due to its low abundance in weaweed, the isolation and purification of eckol are difficult. Its limited availability renders the isolation and purification of eckol labor-intensive processes. Centrifugal partition chromatography (CPC) is an efficient technique for the isolation and purification of eckol. In this study, eckol was isolated from the ethyl acetate fraction of the 70% ethanol extract of E. cava using CPC with a two-phase solvent system of a n-hexane:EtOAc:methanol:water (2:8:3:7, v/v) solution. The purity and anti-inflammatory activity of the isolated eckol were verified by high-performance liquid chromatography and by assaying lipopolysaccharide-induced inflammatory responses in an immortalized murine BV2 microglial cell line, respectively. In conclusion, CPC is a useful technique for simple and efficient isolation of eckol from E. cava.

• Bulletin of the Korean Chemical Society
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• v.29 no.5
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• pp.1043-1047
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• 2008

Simultaneous determination of amitraz, bromopropylate, coumaphos, cymiazole and 2,4-dimethylaniline in 200 honey samples purchased in Korea was performed by reversed-phase high-performance liquid chromatography with multiple UV detection. 2% Acetone in hexane was used for a liquid-liquid extraction and 20-40% water in acetonitrile solutions were used as mobile phases. The LOD for the analytes varied between 0.4 and 1.5 $\mu$g/L and the recoveries were yielded between 64 and 94%. Relative standard deviation of the repeatability of the method is less than 15%. Amitraz was not present in amount above 10 $\mu$ g/L and one for coumaphos and cymiazole and two for bromopropylate, and three for 2,4-dimethylanilne were detected in amount above 10 $\mu$ g/ L. Levels of the acaricide residues found were less than 50 $\mu$ g/L.

• Bulletin of the Korean Chemical Society
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• v.23 no.8
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• pp.1139-1143
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• 2002

Analysis of lysophosphatidic acids (LPAs) is of clinical importance as they can serve a potential marker for ovarian and other gynecological cancers and obesity. It is critically important to develop a highly sensitive and specific method for the early detection of gynecological cancers to improve the overall outcome of this disease. We have established a novel quantification method of LPAs in human plasma by negative ionization tandem mass spectrometry (MS-MS) using multiple reaction monitoring (MRM) mode without the conventional TLC step. Protein-bound lipids, LPAs in plasma were extracted with methanol : chloroform (2:1) containing LPA C14:0 as an internal standard under acidic condition. Following back extraction with chloroform and water, the centrifuged lower phase was evaporated and reconstituted in methanol. The reconstituted solution was directly injected into electrospray source of MS/MS. For MRM mode, Q1 ions selected were m/z 409, 433, 435, 437 and 457 which corresponds to molecular mass [M-H]- of C16:0, C18:2, C18:1, C18:0 and C20:4 LPA, respectively. Q2 ions selected for MRM were m/z 79, phosphoryl product. Using MS/MS with MRM mode, all the species of LPAs were completely separated from plasma matrix without severe interferences. This method allowed simultaneous detection and quantification of different species of LPAs in a plasma over a linear dynamic range of 0.01-25 ㎛olL-1 . The detection limit of the method was 0.3 pmol/mL, with a correlation coefficient of 0.9983 in most LPAs analyzed. When applied to the plasmas of normal and gynecological cancer patients, this new method differentiated two different groups by way of total LPA level.