• Analytical Science and Technology
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• v.24 no.2
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• pp.78-84
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• 2011

The fragmentation patterns of a serine protease inhibitor, camostat, and its degradation product, 4-(4-guanidinobenzoyloxy)phenylacetic acid (GBPA), were for the first time investigated by a triple quadrupole tandem mass spectrometry equipped with an electrospray source (ESI-MS/MS) in positive and/or negative ion mode under collision-induced dissociation (CID). The positive CID spectrum of camostat showed distinctly that the single bond (C-O) cleavage between carbonyl group and oxygen atom of the ester bonds of the compound favorably occurred and then the loss of N,N-dimethylcarbamoylmethyl group was more susceptible than that of guanidine moiety. In the positive ion CID spectrum of GBPA, the initial cleavage between the carbonyl group and oxygen atom of 4-guanidinobenzoyloxy group also occurred, yielding the most abundant fragment ion at m/z 145. On the other hand, the negative CID spectrum of GBPA characteristically showed the occurrence of the most abundant peak at m/z 226 resulting from the sequential neutral losses of $CO_2$ and HN=C=NH from the parent ion at m/z 312.

• Journal of the Korean Applied Science and Technology
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• v.7 no.1
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• pp.93-105
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• 1990

Semicarbazone formation of nine monosubstituted benzaldehydes was studied kinetically in 20% methanol buffer solution at 15, 25, 35, and $45^{circ}C$. The rate of p-nitrobenzaldehyde semicarbazone formation is 2.7 times as fast as that of benzaldehyde, while p-hvdroxybenzaldehyde is 3.6 times as slow as that of benzaldehyde. Activation energies for p-chlorobenzaldehyde, benzaldehyde, p-methylbenzaldehyde, p-methoxybenzaldshyde, p-hydroxybenzaldehyde, and p-dimethylaminobenzaldehyde semicarbazone formation are calculated as 5.80, 6.19, 6.57, 7.06, 8.03, and 6.46 kcal/mol respectively. It is concluded from the effect of ionic strength that the reaction is affected by not ions but neutral molecules involving hydrogen bonding between oxygen atom of carbonyl group and hydrogen atom of acid-catalyst, and concerted attack of the necleophilic reagent, free base on carbonyl compound. Also, the effect of solvent composition is small in 20% and 50% methanol (and ethanol) aqueous solutions. The ${\rho}-{\sigma}$ plots for the rates of semicarbazone formation at pH 7.1 show a linear ${\rho}-{\sigma}$ relationship (${\rho}=0.14l$, in contrast to that at pH 2.75 and pH 5.4 corresponding to ${\rho}-{\sigma}$ correlations reparted by Jencks. The rate of semicarbazone formation at pH 5.4 show a relationship which is convex upward, resulting in a break in the curve but at pH 2.75, slight difference from a linear relationship. As a result of studying citric acid catalysis, second-order rate constants increase linearly with citric acid concentration and show a 2 times increase as the catalyst concentration is varied from 0.025 to 0.1 mol/1 at pH 2,9, but slight increase at pH 5.3. The rate-determining step is addition below pH 5 but is dehydration between pH 5 and 7. Conclusively, the rate-determining step of the reaction changes from dehydration to addition in respect to hydrogen ion activity near pH 5. The ortho: para rate ratio of the hydroxybenzaldehydes for semicarbazone formation is about 17 at $15^{\circ}C$. It is concluded that the results constitute strong evidence in favor of greater stabilization of p- than o-hydroxybenzaldehyde by substituent which donate electrons by resonance and is due to hydrogen bonding between the carbon-bound hydrogen of the-CHO group and the oxygen atom of the substituent.

• Journal of the Korean Society of Food Science and Nutrition
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• v.21 no.5
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• pp.557-565
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• 1992

Volatile components of domestic Meju and Doenjang were extracted by simultaneous steam distillation extraction, and analyzed by GC-MS. Sixty-four kinds of compounds were identified from neutral fraction. The contents of pentanal, hexanal and 1-octen-3-ol were high in cooked soybean while those of 3-methylbutanal and 1-butanol were high in Meju. In the case of Doenjang, so many compounds including acetic acid, ethylester were identified which was not appeared in Meju. The main compounds in Meju were 3-methyl-1-butanol, 2-furancarboxyaldehyde, 1-octen-3-ol, benzeneacetaldehyde, methyloctadecadienoate and methyloctadecenoate. Of the eleven compounds identified from basic fraction, the contents of 2,6-dime-thylpyrazine, trimethylpyrazine and tetramethylpyrazine were high in Meju and Doenjang. Nine kinds of compounds were identified from phenolic fraction and appeared that 4-vinylphenol and p-ethylguaiacol were major compounds in Meju and Doenjang. Fifteen kinds of volatile compounds were contained in acidic fraction. Only four acidic compounds were identified in cooked soybean and Meju, but in Doenjang ten compounds were identified which did not appeared in other samples. Among them pentadecanoic acid was major compound.

• Journal of fish pathology
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• v.21 no.1
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• pp.45-56
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• 2008

This study was conducted to find out biological responses of bivalves exposed to organotin compound.The results of the study confirmed that tribultyltin chloride (TBTCl) induce reduction of survival rate andburrowing activity, and histopathological feature in the foot structure of the equilateral venus, Gomphinaveneriformis. The experimental period was 36 weeks. The experimental groups consisted of a control and 3TBTCl exposure groups (0.4, 0.6, 0.8 ym TBTCl L'). The survival rate and burrowing activity were record-ed daily. For histological analysis, foot tissues were fixed in Bouin' s fluid and then stained H-E stain, AB-PAS (PH 2.5) reaction and Masson's trichrome stain after having serially sectioned the tissue by paraffinmethod at thickness of 4-6 ym. The survival rate was not significantly different between the control andexposure groups for 20 weeks, but in 0.8 Um TBTCl L', it was on the decreased ever since the exposure. Theburrowing activity was not significantly different in the exposure group compared to the control up to 12weeks, but in 0.6 and 0.8 ym TBTCl L', it measured the lowest level after 20 weeks. The foot is composedof the epidermal layer, connective tissue, and muscular layer. The epidermal layer is composed of simplecolumnar, cuboidal epithelia and mucous cells. The cilia were well developed on the apical surface ofepithelium, Circular, longitudinal and transverse muscle bundle were well developed in the muscular layer.The majority mucous cells showed blue color (542c) when it subjected to AB-PAS (PH 2.5) reaction. Nohistopathological alterations in the foot were observed up to 12 weeks. After 20 weeks of exposure to 0.8 (anTBTCl L'', the foot samples of exposed G. veneriformis showed disappearance of cilia and striated borderpartially and extension of hemolymph sinus. The mucous cell increased in the marginal of foot. At 28-weekof exposure to 0.4 ym TBTCl L', it observed weekly acid (564c), neutral (264c) and mixed mucous cell. At36-week of exposure to 0.6 ym TBTCl L', it showed fragmentation of the muscle and collagen fiber bundle,and also diappearance of cilia on epithelia and edema of epithelium in 0.8 ym TBTCl L''.

• Journal of Physiology & Pathology in Korean Medicine
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• v.24 no.6
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• pp.989-995
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• 2010

The aim of this study was to investigate the effect of Taeeumjowuitanggagam-bang(TJV) on the mRNA expression of adipocytokines (TNF-${\alpha}$ and IL-6), and SREBPs. Mice were divided into 4 groups ; a normal group of db/+ mice, a control group of db/db mice, a group (db/db mice) treated with TJV 200 mg/kg, and a group (db/db mouse) treated with TJV 500 mg/kg. They were treated orally with TJV and measured their body weight every other day during 9 weeks. After that, we measured the mRNA expression of adipocytokines (TNF-${\alpha}$ and IL-6) and SREBPs (SREBE-1a and SREBP-1c) in liver, and blood concentration of total cholesterol, triglyceride, too. In addition, liver samples were fixed in 4% PFA for 2 hours and stored in $-70^{\circ}C$. Liver tissues were embedded in Optical cutting temperature(OCT) compound and 30 ${\mu}m$ sections were cut. Tissue sections were stained Oil-Red-O to visualize neutral lipids. Nuclei were stained with hematoxylin solution. In result, the TJV reduced the mRNA expressions of TNF-${\alpha}$ and IL-6 and SREBPs in liver and stained liver tissue less red than control group. However, there was no significant differences in total cholestreol and triglyceride blood concentration and body weight among groups. The TJV has inhibitory effect on the mRNA expression of adipocytokines and SREBPs. Therefore, it is assumed that the TJV is related to inhibiting lipogenesis in the liver

• Journal of Life Science
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• v.17 no.2 s.82
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• pp.286-292
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• 2007

Free amino acids and volatile compounds of fresh garlic and its liqueur were investigated to search elution profile of those components as basic data for development of garlic liqueur. The garlic was soaked in 20% alcohol solution and then sampled every week for 5 weeks. The major free amino acids were L-aspartic acid, L-glutamic acid, L-arginine, L-alanine, L-proline, L-asparagine and L-serine. Neutral amino acids such as L-threonine, L-proline, L-valine and L-leucine, and aromatic amino acids such as tyrosine and phenylalanine were eluted over 80% of those content in fresh garlic after 3 weeks of soaking, but acidic, basic and sulfur containing amino acids were below 80% even after 5 weeks. Sulfide compounds such as diallyl trisulfide, diallyl disulfide, methyl allyl disulfide, 2-vinyl-4H-1,3-dithi in, 3-vinyl-3,4-dihydro-1,2-dithiin, 3,5-diethyl-1,24-trithiolane, isobutyl isothiocyanate and diallyl sulfide were identified as major volatile compounds of fresh garlic by using GC/MS. Among volatile compounds of fresh garlic, allyl alcohol, diallyl disulfide, 3,5-diethyl-1,2,4-trithiolane, diallyl trisulfide and 3,4-dimethoxy furan were eluted to liqueur, but those compounds except 3,5-diethyl-1,2,4-trithiolane were lowered in liqueur during soaking. Furfural, 5-methylfurfural, 5-hydroxymethylfurfural, dimethyl pyrazine, furfuryl alcohol, 3-hydroxy-2-bytanone and 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyr-an-4-one were generated newly and their content increased in liqueur during soaking.

• Korean Journal of Plant Resources
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• v.26 no.4
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• pp.426-432
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• 2013

The results of the content of total polyphenol and flavonoid, DPPH (1-1-diphenyl-2-picryl-hydrazyl) radical scavenging activity, ABTS [2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid)] radical scavenging activity, nitrite scavenging activity and SOD-like activity of methanol extracts from immature cotton boll are follows. The contents of total polyphenol and flavonoid compound were higher in small size cotton boll, and DPPH and ABTS radical scavenging activity also showed a relatively high activity in the small size. These results indicate that there is a correlation between phenol content and DPPH radical scavenging, ABTS radical scavenging. The test concentrations of immature cotton boll extract for measuring DPPH and ABTS radical scavenging activities were set as 1.25, 2.5, 5, 10 and 20 mg/ml. Immature cotton boll has high radical scavenging activity at the concentration of 1.25~20 mg/ml and the result showed a tendency to increase in a concentration-dependent. The nitrite scavenging activity showed high activity in the pH 1.2, and the result in the pH 4.2 showed progressively less active, and in the pH 6.0 near neutral was confirmed that does not affect the nitrite scavenging. In addition, SOD-like activity showed somewhat lower activity compared with ascorbic acid, but tended to be higher when compared with the results of the other natural substances. Through this experiment, we confirmed that immature cotton boll was excellent antioxidant activity. Therefore, it is demonstrated that the cotton suggest the possibility of development of new material for cosmetic product or functional food in the future, and is expected to make a greater usability.

• Journal of the Korean Chemical Society
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• v.50 no.4
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• pp.315-320
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• 2006

manganese oxides have been prepared by Chimie Douce redox reaction between permanganate and chalcogen element fine powder under acidic condition (pH = 1). According to powder X-ray diffraction analyses, the S- and Se-doped manganese oxides are crystallized with layered birnessite and tunnel-type -MnO2 structures, respectively. On the contrary, Te-doped compound was found to be X-ray amorphous. According to EDS analyses, these compounds contain chalcogen dopants with the ratio of chalcogen/manganese = 4-7%. We have investigated the chemical bonding character of these materials with X-ray absorption spectroscopic (XAS) analysis. Mn K-edge XAS results clearly demonstrated that the manganese ions are stabilized in octahedral symmetry with the mixed oxidation states of +3/+4. On the other hand, according to Se K- and Te L1-edge XAS results, selenium and tellurium elements have the high oxidation states of +6, which is surely due to the oxidation of neutral chalcogen element by the strong oxidant permanganate ion. Taking into account their crystal structures and Mn oxidation states, the obtained manganese oxides are expected to be applicable as electrode materials for lithium secondary batteries.

• Journal of the Korean Chemical Society
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• v.55 no.4
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• pp.594-602
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• 2011

The effect of ${\alpha}$-, ${\beta}$- and ${\gamma}$-picolines on the stereochemistry of the coordination compounds of lanthanide(III) nitrates derived from 4[N-(furfural)amino]antipyrine semicarbazone (FFAAPS) has been studied. The general composition of the present coordination compounds is [Ln(FFAAPS)$(NO_3)_3$Pic] (Ln=La, Pr, Nd, Sm, Gd, Tb, Dy or Ho and Pic=${\alpha}$-, ${\beta}$- or ${\gamma}$-picolines). All these coordination compounds have been characterized by elemental analyses, molecular weight, molar conductance, magnetic susceptibility, infrared and electronic spectra. The infrared studies suggest that the FFAAPS behaves as a neutral tridentate ligand with N, N, O donor while ${\alpha}$-, ${\beta}$- or ${\gamma}$-picoline is coordinated to the lanthanide(III) ions via heterocyclic N-atom. Nitrates are bicovalently bonded in these compounds. From the electronic spectral data, nephelauxetic effect (${\beta}$), covalence factor ($b^{1/2}$), Sinha parameter (${\delta}%$) and the covalence angular overlap parameter (${\eta}$) have been calculated. Thermal stabilities of these complexes have been studied by thermogravimetric analysis. The coordination number of lanthanide(III) ions in the present compound is found to be ten. The antibacterial studies screening of the primary ligand FFAAPS and the complexes showed that the present complexes have moderate antibacterial activities.

• KSBB Journal
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• v.21 no.3
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• pp.181-187
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• 2006

In this study, problems related with pH control in electrokinetic(EK) bioremediation of phenanthrene contaminated soil were observed, and the effects of pH control methods on the removal efficiency were investigated to search a further application strategy. In a preliminary experiment, it was found out by flask cultivation that a certain sulfate concentration was needed to degrade phenanthrene well using Sphingomonas sp. 3Y. However, when $MgSO_4$ was used as sulfate source in EK bioremediation, the bacterial activity reduced seriously due to the abrupt decrease of pHs in soil and bioreactor by the combination of magnesium and hydroxyl ions. When another strong buffering compound was used to control the pH problem, the good maintenance of the bacterial activity and pHs could be observed, but the removal efficiency decreased largely. When a low concentration of $MgSO_4$ was added, the removal efficiency decreased somewhat in spite of the good maintenance of neutral pHs. With the addition of NaOH as a neutralizing agent, the removal efficiency also decreased because of the increase of soil pH. Consequently the selection of electrolyte composition was a very important factor in EK bioremediation and some sulfate sources suitable for both bacterial activity and contaminant degradation should be investigated.