• Journal of Pharmaceutical Investigation
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• v.21 no.2
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• pp.67-71
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• 1991

A simple and sensitive method was developed for the quantification of free and conjugated bile acids in bezoar without prior hydrolysis. $3{\alpha}-Hydroxy$ bile acids are first oxidized to 3-keto bile acids in the reaction catalyzed by $3{\alpha}-hydroxysteroid$ $dehydrogenase(3{\alpha}-HSD)$. During this oxidative reaction, an equimolar quantity of nicotinamide adenine dinucleotide(NAD) is reduced to NADH and subsequently oxidized to NAD with concomitant reduction of nitrotetrazolium blue(NTB) to diformazan by the catalytic action of diaphorase. The diformazan has an absorbance maximum at 540 nm. The intensity of the color produced is directly proportional to bile acids concentration in the bezoar extracts. The optimum conditions for the enzymatic reaction such as effects of reaction time, reaction temperature and pH, and stability were investigated. Calibration plots for the sodium chelate observed to be linear and intra-, inter-assay analytical recovery of bile acids averaged $97.65{\pm}3.4%(S.D.)$. Therefore, it is considered that the quality control of total bile acids from bezoar or bezoar-containing liquid preparation using this simple and sensitive assay system will be acceptable. Also current bezoars and bezoar-containing liauid preparations were examined their total bile acids from this method.

• Analytical Science and Technology
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• v.6 no.5
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• pp.417-424
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• 1993

Eight-coordinate tetrakis molybdenum(IV) complexes containing 5,7-dichloro-8-hydroxyquinolinol(Hdcq) and 2-mercaptopyrimidine(Hmpd) has been prepared. $Mo(mpd)_4$, $Mo(dcq)(mpd)_3$, $Mo(dcq)_2(mpd)_2$, $Mo(dcq)_3(mpd)$ and $Mo(dcq)_4$ complexes have been isolated by thin-layer chromatography on silicagel plates. These complexes have been charaterized by $^1H-nmr$ spectrum and UV-Vis. spectrum. The chemical shift values of the protons ${\alpha}$ to the nitrogen in the ligands are shifted to down field. The relative intensities of the peaks which are positioned at the same proton of $Mo(dcq)(mpd)_3$ and $Mo(dcq)_3(mpd)$ are observed in 2:1 ratio, in case of $Mo(dcq)_2(mpd)_2$ appears in approximately a 1:1 ratio. The stereochemistry of the complexes in discussed in terms of their nmr spectrum and Orgel's rule. By vertue of the intensities (${\varepsilon}$>10,000~25,000) the low energy($16,600{\sim}19,800cm^{-1}$) bands are observed for the electronic spectra of the complexes are assigned as charge transfer bands.

• The Korean Journal of Nuclear Medicine
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• v.29 no.1
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• pp.110-117
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• 1995

Tc-99m Labeled hexamethylenepropyleneamineoxime ([$^{99m}Tc$]-HMPAO) is a famous amino-oxime compound and is widely used to construct SPECT images of cerebral blood flow. To investigate the relationship between chemical structure and radiolabeling in these kind of diamine-oxime compounds, we synthesized seven compounds by Schiff's base formation and successive reduction with sodium borohydride. They were (RR/SS )-4,8-diaza-3,6,6,9-tetramethylundecane-2,10-dione bisoxime (2), (RR/SS/meso)-4,8-diaza-3,9-dimethy-lundecane-2,10-dione bisoxime (4), (RR/SS/meso)-4,8-diaza-3,10-dimethyldodecane-2,11-dione bisoxime (5), (RR/SS/meso)-4,7-diaza-3,6,6,8-tetramethyldecane-2,9-dione bisoxime (8), (RR/SS/meso)-4,7-diaza-5,6-cyclohexyl-3,8-dimethyldecane-2,9-dione bisoxime (10), (RR/SS/meso)-3,4-bis(1-aza-2-methyl-3-oxime-1-butyl)-benzoic acid (12), and (RR/SS/ meso)-2,3-bis(1-aza-2-methyl-3-oxime-1-butyl) benzophenone (14). Chemical structures of all the synthesized compounds were identified by taking $^1H$ spectrum. Among them, 2 and 4 are propyleneamine oxime (PnAO), 6 is butyleneamine oxime (BnAO) and 8, 10, 12 and 14 are ethyleneamine oxime (EnAO). Each compound (0.5 mg) was incubated with stannous chloride (0.5 g - 8 g), carbonate-bicarbonate buffer (final concentration = 0.1 M, pH 7 - pH 10) and Tc-99m-pertechenate (1 ml). Tc-99m labeling of these compounds were checked by ITLC (acetone), ITLC (normal saline), reverse phase TLC (50 % acetonitrile) and ITLC (ethyl acetate). According to the results, EnAO's were not labeled by Tc-99m in any of above condition. About 11 % of maximum labeling efficiency was obtained with BnAO. However, 4 (PnAO) was labeled with Tc-99m to 85 % which is similar to the labeling efficiency of 2 (HMPAO). Hydrophilic impurity (9 % ) was the most significant problem with the labeling of 4, however, pertechnetate (3 % ) and colloid (3 %) were minor problem. In conclusion, we synthesized seven diamine blsoxlme compounds. Among them, four EnAO compounds were not labeled by Tc-99m. A BnAO was labeled poorly and two PnAO's were labeled well. These labeling can be explained by tertiary structure of their Tc-99m chelate.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.32 no.2
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• pp.121-126
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• 1999

In order to degrade chitin by enzymatic hydrolysis, it is required from screening highly active deacetylase. To this end, we examined three fungal strains and it turned out that Mucor rouxii produced highly active deacetylase, this enzyme exhibited the highest enzymatic activity against colloidal chitin. The conditions for growing Mucor rouxii are as follows; the effective carbon source, nitrogen source, adequate initial pH, temperature and incubation time were $2\%$ glucose, $1.33\%$ yeast extract, $0.66\%$ pepton, 4.5, $25{\pm}2^{\circ}C$ and 48hr, respectively. The optimum pH and temperature for purified enzyme activity were 5.5 and $40^{\circ}C$, respectively. The purified enzyme was stable at pH ranging from 4.5 to 5.5. However, the enzyme activity was decreased to less than $50\%$ at pH blow 45 and above 7.5. At temperatures above $50^{\circ}C$, the enzyme activity was decreased remarkably. The enzyme was inhibited by LiC1, $HgCl_2$, and $BaCl_2$, but stimulated by $CaCl_2$ and $ZnC1_2$, The activity of purified enzyme was increased by L-cysteine and 2-mercaptoethanol, while decreased by O-phenanthroline, p-CMB, EDTA, and iodoacetate. The $K_m$ and the $V_{max}$ value of purified enzyme were $1.2\%$ and 59.5 U/mg, respectively. The deacetylation activity of purified enzyme was not detected at optimal reaction condition when chitin particle suspension was used.

• Journal of the Korean Chemical Society
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• v.44 no.5
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• pp.403-409
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• 2000

The formation and dissociation rates of $Zn^{2+}$ Complexes with l,4,7,10-tetraaza-13,16-diox-acyclooctadecane-N,N',N",N'"-tetraacetic acid (1), 1,4,7,10-tetraaza-13,16- dioxacyclooctadecane-N,N',N",N'"-tetramethylacetic acid (2), and 1,4,7,10-tetraaza-13,16- dioxacyclooctadecane-N,N',N",N'"-tetrapropionic acid(3) have been measured by stopped-flow and conventional spectrophotometry. Observations were made at 25.0$\pm$0.1 $^{\circ}C$ and at an ionic strength of 0.10 M NaClO$_4$. The formation reactions of $Zn^{2+}$ ion with 1 and 2 took place by the rapid formation of an intermediate complex (ZnH$_3L^+$) in which the $Zn^{2+}$ ion is incompletely coor-dinated. This might then lead to be a final product in the rate-determining step.ln the pH range 4.76-5.76, the diprotonated (H2L2-) form is the kinetically active species despite of its low concentration. The stability con-stants (log$K_{(ZnH$_3$3$L^+$)}$) and specific water-assisted rate constants (koH) of intermediate complexes have been deter-mined from the kinetic data. The dissociation reactions of $Zn^{2+}$ complexes of 1,2, and 3 were investigated with $Cu^{2+}$ ions as a scavenger in acetate buffer. All complexes exhibit acid-independent and acid-catalyzed con-tributions. The effect of buffer and $Cu^{2+}$ concentration on the dissociation rate has also been investigated. The ligand effect on t dissociation rate of $Zn^{2+}$ complexes is discussed in terms of the side-pendant armsand the chelate ring sizes of the ligands.

• Journal of the Korean Chemical Society
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• v.16 no.5
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• pp.314-319
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• 1972

N-Methyl-p-aminophenol was polymerized by oxidative couplng in the aqueous iron chelate solution in the presence of oxygen, and black precipitate of oligo-(N-methyl-p-aminophenol) was formed quantitatively. In this oxidative polymerization reaction, methyl group attached to N in the monomer was partly eliminated, and it was clarified by the infrared spectra from the fact that the absorption of ${\delta}\;asym\;CH_3\;1460\;cm^{-1}$ and ${\delta}\;sym\;CH_3\;1380\;cm^{-1}$ in acetone insoluble fraction was much weaker than that in acetone soluble fraction. From Thermo-gravimetric analysis, oligo-(N-methyl-p-aminophenol) showed about 40% weight loss at $600^{\circ}C$ and it was less heat-resistant than oligo (p-aminophenol) that methyl group was not contained. In pyrolysis of oligo-(N-methyl-p-aminophenol) in He atmosphere, monomer N-methyl-p-aminophenol and water were formed, and in the pyrolytic gases, $H_2,\;CO,\;CO_2$ were detected by gas chromatography. From the above facts, to the structural change on oligo-(N-methyl-p-aminophenol) when it was heat-treated, it was considered that original linear structure was partly degraded, and the most of the oligomer was to go in with melt polycondensation to form polymer, and heat-resistant cyclic structure was formed at a time.

• Journal of the Korean Chemical Society
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• v.37 no.7
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• pp.655-661
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• 1993

The neutral monomeric compounds $[Mo(NO)_2Cl_2(phen)]$ and $[W(NO)_2Cl_2(phen)]$ (phen= 1,10-phenanthroline) have been prepared by reactions of polymeric compounds $[{Mo(NO)_2Cl_2}n],\;[{W(NO)_2Cl_2}n]$ with chelate ligands. Additions of one equivalent of silver(I) perchlorate to these cis-dinitrosyl compounds in acetone solution produce $[Mo(NO)_2(phen)(S)Cl][ClO_4]\;and\;[W(NO)_2(phen)(S)Cl][ClO_4]$ (S = acetone). The homo- and hetero-dinuclear complexes, $[Cl(phen)(NO)_2M(pyz)M'(NO)_2(phen)Cl][ClO_4]_2$ (M = Mo, W) and $[Cl(phen)(NO)_2M(pyz)M'(NO)_2(phen)Cl][C1O_4]_2$ (M = Mo, M' = W) have been prepared by these monocationic complexes with pyrazine ligand respectively. These complexes characterized by elemental analysis, $1^H-\;and\;^{13}C-NMR$, infrared, and UV-visible spectroscopy are reported. The spectral data indicate that homo- and hetero-dinuclear complexes were symmetrical structures of $C_{2v}$.

• Food Science of Animal Resources
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• v.28 no.4
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• pp.408-414
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• 2008

Low-fat sausages (LFS) containing various levels (0, 0.3, and 0.6%) of activated lactoferrin (ALF) which was prepared by dialysis to chelate irons of native lactoferrin, were manufactured and measured the physicochemical and textural properties, and shelf-life effect during refrigerated storage ($8^{\circ}C$). LFSs contained 72-16% moisture, 1-2% fat, 12-14% protein and a pH range of 6.04-6.08. No differences in physico-chemical and textural properties were observed with the increased ALF (p>0.05). Microbial growth of Listeria monocytogenes (LM), which inoculated at the levels of $10^4$ CFU/g, was increased with increased storage time. ALF at the amount of 0.6% slightly inhibited the microbial growth on the LFS (p<0.05), as compared to those of LFSs without ALF, however it had lower antimicrobial activity than those of 3.3% sodium lactate. These results indicated that the addition of ALF at the level of 0.6% affected the antibacterial activity of LFSs, resulting in the suppression of microbial growth in LFSs without quality defects.

• Asian-Australasian Journal of Animal Sciences
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• v.14 no.12
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• pp.1734-1740
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• 2001

Feeding trials using weanling pigs and broiler chicks were conducted to evaluate the efficacy of different metal-amino acid chelates and complexes at various levels of copper and zinc on the performance and fecal excretions. A total of 200 weanling pigs (Large White ${\times}$ Yorkshire ${\times}$ Duroc, $11.20{\pm}0.81kg$) were randomly assigned to 5 dietary treatments following a randomized complete block design. Each treatment was replicated 4 times with 10 pigs per pen. The dietary treatments were designated as : A-diet containing 170 ppm Cu from $CuSO_4$ and 120 ppm Zn from $ZnSO_4$, B-diet containing 85 ppm Cu from Cu-amino acid chelate (CAC) and 60 ppm Zn from Zn-amino acid chelate (ZAC), C-diet containing 170 ppm Cu from CAC and 120 ppm Zn from ZAC, D-diet containing 85 ppm Cu from Cu-lysine complex (CL) and 60 ppm Zn from Zn-methionine complex (ZM), and E-diet containing 170 ppm Cu from CL and 120 ppm Zn from ZM. On the other trial, 144 of one day old broiler chicks were randomly distributed to 6 dietary treatments following a completely randomized design. Each treatment was replicated 3 times with 8 chicks per replicate. The dietary treatments were as follows: 1-diet with 60 ppm Cu from $CuSO_4$ and 40 ppm Zn from $ZnSO_4$, 2-diet with 120 ppm Cu from $CuSO_4$ and 80 ppm Zn from $ZnSO_4$, 3-diet with 60 ppm Cu from CAC and 40 ppm Zn from ZAC, 4-diet with 120 ppm Cu from CAC and 80 ppm Zn from ZAC, 5-diet with 60 ppm Cu from CL and 40 ppm Zn from ZM, and 6-diet with 120 ppm Cu from CL and 80 ppm Zn from ZM. In Exp. 1 with pigs, there was no difference on average daily gain and average daily feed intake observed among treatments. There was improvement (p<0.05) on the overall feed conversion ratio (FCR) of pigs fed diet containing 120 ppm Zn and 170 ppm Cu from metal-amino acid chelates relative to those fed diet containing inorganic sources of Cu and Zn but equally efficient as those fed diet containing metal-amino acid complexes. Pigs fed diet containing either metal-amino acid chelates or complexes as sources of Cu and Zn had higher (p<0.05) Cu and Zn concentration in serum and lower (p<0.05) in feces than those receiving diet with inorganic sources. In Exp. 2 with broiler chicks, the overall FCR was not different among treatments. Higher (p<0.05) Cu and Zn concentration in serum was obtained from birds fed diet with 60 ppm Cu and 40 ppm Zn from metal-amino acid chelates compared to those fed diet with inorganic sources of Cu and Zn. Also, the feces collected from birds fed diet with either metal-amino acid chelates or complexes contained generally lower Cu and Zn than those birds fed diet with inorganic sources. The higher the dietary level of Cu and Zn the higher the Cu and Zn concentration in the feces. Based on the results, both metal-amino acid chelates and complexes of Cu and Zn at low levels (Zn 60 ppm, Cu 85 ppm for weanling pigs and Zn 40 ppm, Cu 60 ppm for broiler chicks) are not different from that of high levels of inorganic sources in maintaining growth performance and serum concentration. The fecal excretions for Cu and Zn were greatly reduced when organic sources were used.

• Investigative Magnetic Resonance Imaging
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• v.10 no.1
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• pp.20-25
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• 2006

Purpose : To evaluate the NMR relaxation properties of newly developed high performance paramagnetic complexes. Materials and methods : 4-aminomethylcyclohexane carboxylic acid (0.63g, 4 mmol) was mixed with the suspension solution of DMF (15mL) and DTPA-bis-anhydride (0.71g, 2 mmol) to synthesize the ligand. The ligand was then mixed with Gd2O3 (0.18g, 0.5 mmol) to synthesize Gd-chelate. For the measurement of magnetic relaxivity of paramagnetic compounds, the compounds were diluted to 1mM and then the relaxation times were measured at 1.5T(64 MHz). Inversion-recovery pulse sequence was employed for T1 relaxation measurement and CPMG(Carr-Purcell-Meiboon-Gill) pulse sequence was employed for T2 relaxation measurement. Using MATLAB(Version 7.1) program, T1 magnetic relaxation map, R1 map, T2 magnetic relaxation map and R2 map were developed to represent magnetic relaxation time and magnetic relaxivity as image. Results : Compared to $R1=4.9mM^{-1}sec^{-1}$ and $R2=4.8mM^{-1}sec^{-1}$ of Omniscan (Gadodiamide), which is commercially available paramagnetic MR agent, R1 of SUK090(Gd-C32H74N5O24) was $12.46mM^{-1}sec^{-1}$ and R1 of SUK091(Gd-C34H78N5O24) was $12.77mM^{-1}sec^{-1}$. However, R1 of SUK092(Gd-C30H56N5O17) was decreased to $2.09mM^{-1}sec^{-1}$. In case of R2, SUK090(Gd-C32H74N5O24) was $8.76mM^{-1}sec^{-1}$ and SUK091(Gd-C34H78N5O24) was $7.60mM^{-}1sec^{-1}$ whereas SUK092(Gd-C30H56N5O17) was decreased to $1.82mM^{-1}sec^{-1}$. Conclusion : Among three new paramagnetic complexes, SUK090(Gd-C32H74N5O24) and SUK091(Gd-C34H78N5O24) showed higher T1, T2 magnetic relaxation rates than that of commercially available paramagnetic MR agent and thus expected to have more contrast enhancement effect.