3,3-dichlorobenzidine is suspected to be cancinogenic in experimental animal and human. Several studies have investigated excretion of metabolites in urine, hemoglobin adduction and cancer incidence among workers occupationally exposed to 3,3'-dichlorobenzidine. In these researches, metabolites of 3,3'-dichlorobenzidine had a very important role, and were required as highly purity. The purpose of this study was synthesis and isolation of its metabolites from 3,3'-dichlorobenzidine. 3,3'-dichlorobenzidine was partially dissolved in benzene, ether, ethanol and methanol, and completely dissolved in 70% acetic acid on mixtures of citric acid containing less than 1% DCB, pyridine, a mixture of 0.5N NaOH and toluene(1:2), and phenol saturated with 20 mM TRIZA base. DCB, monoacetyl-DCB and diacetyl-DCB were measured by using gas chromatography/mass spectrometry(GC/MS). Detection for checking them was nitrogen phosphorous detection mode(NPD), and for identifying them was selected ion monitoring mode(SIM). The base peaks were 252 m/z in DCB, 252, and 294 m/z in monoacetyl-DCB, and 252, 294 and 336 m/z in diacetyl-DCB, respectively. Diacetyl-DCB was synthesized by titrating DCB solution of pyridine with sufficient acetyl chloride. Precipitation was diacetyl-DCB, which was purity of 98.7%. And its supernatant was composed of DCB, monoacetyl-DCB and diacetyl-DCB. By using acetic acid as controller of acetylation, monoacetyl-DCB was isolated from diacetyl-DCB . And residual pyridine was removed by using acetone. The purity of monoacetyl-DCB was 98.8%.
Kim, Ho Soo;Lee, Chan-Ju;Kim, So-Eun;Ji, Chang Yoon;Kim, Sung-Tai;Kim, Jin-Seog;Kim, Sangyong;Kwak, Sang-Soo
Journal of Plant Biotechnology
/
v.45
no.3
/
pp.190-195
/
2018
Sweetpotato [Ipomoea batatas (L.) Lam] represents an attractive starch crop that can be used to facilitate solving global food and environmental problems in the $21^{st}$ century. It can be used as industrial bioreactors to produce various high value-added materials, including bio-ethanol, functional feed, antioxidants, as well as food resources. The non-profit Center for Science in the Public Interest (CSPI) announced sweetpotato as one of the ten 'super foods' for better health, since it contains high levels of low molecular weight antioxidants such as vitamin-C, vitamin-E and carotenoids, as well as dietary fiber and potassium. The United States Department of Agriculture (USDA) also reported that sweetpotato is the best bioenergy crop among starch crops on marginal lands, that does not affect food security. The Food and Agriculture Organization (FAO) estimated that world population in 2050 will be 9.7 billion, and require approximately 1.7 times more food than today. In this respect, sweetpotato will be a solution to solving problems such as food, energy, health, and environment facing the globe in the $21^{st}$ century. In this paper, the current status of resources, and cultivation of sweetpotato in the world was first described. Development of a new northern route of the sweetpotato and its prior tasks of large scale cultivation of sweetpotato, were also described in terms of global food security, and production of high-value added biomaterials.
Stroke is a serious disease despite recent improvement in medical and surgical treatment. Hence, identification of modifiable risk factors for stroke is important. This case-control study was done to demonstrate that relationship between smoking, alcohol consumption, obesity, perception of saltness and the incidence of stroke and to identify that smoking, alcohol consumption, obesity and perception of saltness, after adjusting for age, hypertension. A structured interview was carried out from April 15, 1996 to May 3, 1996 in Yonsei Medical Center. The study group consisted of 59 neurologically confirmed stroke patients as the study group and 59 non-stroke patients as controls. Analysis of the data was done by means of ${\chi}^2$-test and logistic regression analysis. The results were as follows. In the study group: 1) Hypertension in males had a 10.2 odds ratio (p<0.05), cardiovascular disease in females had a 11.3 odds ratio (p<0.05) and a farnily history of stroke in males had a 3.1 odds ratio (p<0.05). 2) Females smoking one or more cigarettes had a 8.3 odds ratio (p<0.1), but males had no direct relationship with odds ratio of 1.5 (non-significant). 3) Alcohol consumption in males had a 0.4 odds ratio, and in females had a 0.8 odds ratio. The odds ratio was decreased in alcohol consumption group (non-significant). 4) Males with more than 20 cigarettes pack-years history had a 2.5 odds ratio (p<0.05), more than 25 Body Mass Index had a 3.1 odds ratio (p<0.05) and more than 220 ml ethanol weekly consumption had a 1.5 odds ratio (non-significant). 5) Female smokers had a 8.3 odds ratio (p<0.1), drinkers a 0.8 odds ratio and more than 25 Body Mass Iidex, a 43.1 odds ratio (p<0.05). 6) Females without saltness perception from a 0.5% salt solution had a 6.8 odds ratio (non-significant). 7) By logistic regression analysis independent risk factors for stroke in males were found to be hypertention, age, and obesity. The study was limited because number of subjects was too small for practical implications. However, like as other results, this study suggest that people should be advised to control hypertension, and obesity since these carry a risk of stroke.
Journal of the Korean Applied Science and Technology
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v.7
no.1
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pp.93-105
/
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.24
no.2
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pp.323-329
/
1995
For the effective utilization of dark meat separated as by-product from skip-jack canning, the dark meat concentrate(DPC) was prepared by removal of extractable materials with ethanol from dried dark meat. Dark meat protein hydrolysate(DPH) was prepared by the hydrolysis of DPC with ${\alpha}-chymotrypsin$. ${\alpha}-Chymotrypsin$ hydrolysed DPC to the extend of 79% during 10hr. The solubility over a pH range 1~12 showed similar trend on the both of DPH and DPC. The highest solubility was 81% on the DPH and was 36% on the DPC at pH 3. The lowest solubility was 65% on the DPH and was 22% on the DPC at pH 7. The content of total free amino acid was higher in the DPC than in the DPH, but the content of total essential free amino acid was higher in the DPH. Especially, the contents of taurine in the DPC and DPH were much higher than those of other amino acids. The result of sensory evaluation on the fish sauce analogue showed good taste, color and odor at the supplemented level of 8g DPH per 100ml of raw solution of fish sauce analogue and didn't show signifcaint difference compared with market fish sauce(p<0.05). On the preparation of surimi gel, 2% substitution of DPH for the supplemented starch was the most appropriate level.
The facile route of preparing S-2-(${\omega}$-aminoalkylamino) ethyl dihydrogen phosphorothioates, potential chemical radioprotectants, have been studied. Intermediate 3-(2-phthalimidoethyl)-2-oxazolidinone was prepared by a reaction of potassium phthalimide and 3-(2-bromoethyl)-2-oxazolidinone, which was obtained through the alkaline ring closure of a mixture of carbonate and 2,2'-dibromo diethylamine prepared from diethanolamine. This was converted to N-[2-(2-bromoethylamino)ethyl] phthalimide hydrobromide by 30% HBr(gas) in acetic acid and N-(2-bromoethyl)-1,2-ethanediamine dihydrobromide was obtained by reacting the hydrobromide with a solution of HBr-HOAc. N-(2-bromoethyl)-1,3-propanediamine dihydrobromide could be prepared through the Cortese treatment of 2-(3-aminopropylamino) ethanol, which was prepared by a reaction of 1,3-diaminopropane and 2-chloroethanol. These dihydrobromides were treated by sodium thiophosphate in DMF to result S-2-(${\omega}$-aminoalkylamino) ethyl dihydrogen phosphorothioates. The characteristics of each reaction path were discussed in regards to reaction conditions and overall yields and a facile route of preparing each derivative was proposed.
Jo, Yejin;Seo, Yeong-Hui;Jeong, Sunho;Choi, Youngmin;Kim, Eui Duk;Oh, Seok Heon;Ryu, Beyong-Hwan
Korean Journal of Materials Research
/
v.25
no.12
/
pp.719-726
/
2015
For a decade, solution-processed functional materials and various printing technologies have attracted increasingly the significant interest in realizing low-cost flexible electronics. In this study, Cu nanoparticles are synthesized via the chemical reduction of Cu ions under inert atmosphere. To prevent interparticle agglomeration and surface oxidation, oleic acid is incorporated as a surface capping molecule and hydrazine is used as a reducing agent. To endow water-compatibility, the surface of synthesized Cu nanoparticles is modified by a mixture of carboxyl-terminated anionic polyelectrolyte and polyoxylethylene oleylamine ether. For reducing the surface tension and the evaporation rate of aqueous Cu nanoparticle inks, the solvent composition of Cu nanoparticle ink is designed as DI water:2-methoxy ethanol:glycerol:ethylene glycol = 50:20:5:25 wt%. The effects of poly(styrene-co-maleic acid) as an adhesion promoter(AP) on rheology of aqueous Cu nanoparticle inks and adhesion of Cu pattern printed on polyimid films are investigated. The 40 wt% aqueous Cu nanoparticle inks with 0.5 wt% of Poly(styrene-co-maleic acid) show the "Newtonian flow" and has a low viscosity under $10mPa{\cdots}S$, which is applicable to inkjet printing. The Cu patterns with a linewidth of $50{\sim}60{\mu}m$ are successfully fabricated. With the addition of Poly(styrene-co-maleic acid), the adhesion of printed Cu patterns on polyimid films is superior to those of patterns prepared from Poly(styrene-co-maleic acid)-free inks. The resistivities of Cu films are measured to be $10{\sim}15{\mu}{\Omega}{\cdot}cm$ at annealing temperature of $300^{\circ}C$.
Because of high contents of cellulose (~37 wt%) and hemicellulose (~17%), rice straw seems to be a potential lignocellulosic biomass for production of bioethanol. In this study, Ammonia Recycled Percolation (ARP) pretreatment of rice straw was extensively investigated. In particular, the experimental study included the effects of temperature, reaction time and concentration of ammonia on compositions and enzymatic digestibility of the resulting solid residues; the ranges of pretreatment conditions were, in turn, $150{\sim}190^{\circ}C$, 10~90 min and 0~20 wt%. Through ARP pretreatment, the lignin content was reduced by as high as ~84% while 20~80% of the hemicellulose was also solubilized. The solid residue resulted from the pretreatment with 15 wt% aqueous ammonia solution at $170^{\circ}C$ for 90 mim showed as high as ~90% of digestibility with 15FPU/g of glucan enzyme loading. Supplement of xylanese to cellulase led to a notable enhancement of digestibility, indicating a discernable inhibitory role of hemicellulose. Simultaneous Saccharification and Fermentation (SSF) and Simultaneous Saccharification and Co-Fermentation (SSCF) were performed to obtain ethanol productions of 13.8 g/L (corresponding to 81% yield) and 15 g/L (corresponding to 89% yield), respectively.
We purified and characterized a crude polysaccharide from Spirodela polyrhiza with anti-complement activities. The crude polysaccharide fraction (SP-0) which had potential anti-complement activity was extracted in hot water for 4 hrs at 10$0^{\circ}C$. The ethanol-precipitate, the crude polysaccharide traction (SP-1), showed a potent anti-complement activity. Further purification of the crude polysaccharide (SP-1) was carried out by cetavlon, ion exchange chromatography and gel column chromatography. Among cetavlon fractions, SP-4 showed the most potent anti-complement activity. When 100 $\mu\textrm{g}$/mL of SP-4 was incubated with an equal volume of normal human serum (NHS), the TCH$_{50}$ was reduced by about 78%. When the SP-4 fraction was further purified by DEAE-Sepharose (Cl$^{[-10]}$ ), the SP-4IIa, SP-4IIb and SP-4IIc, absorbed fractions, were almost the same as the anti-complement activities of SP-4. SP-4IIc, having the greatest potential activation and the highest yield by ion exchange chromatography, was further purified by gel column chromatography on a Sepharose CL-6B column. Four polysaccharide fractions of SP-4IIc-1, SP-4IIc-2, SP-4IIc-3 and SP-4IIc-4 were obtained, consisting mainly of arabinose, rhamnose, galactose and glucose, with approximate molecular weights of about 305,000, 132,000, 64,000 and 12,000, respectively. Among these subfractions, SP-4IIc-1 had the most potent anti-complement activity. When the SP-4IIc-1 aggregate was applied to a gel column chromatography in 10 mM and 50 mM NaCl solution, the position of the peak fractions shifted to a low molecular weight region, and the molecular weight of SP-4IIc-1 decreased with increased NaCl concentration in the gel column chromatography. It was found that the self-aggregation formed spontaneously in void volume by gel column chromatography using Sepharose CL-6B in water and the self-aggregation significantly affected the anti-complement function.
A precursor of lithium manganese oxide was synthesized by mixing $(CH_3)_2CHOLi\;with\;Mn(CH_3COO)_2{\cdot}4H_2O$ in ethanol using a sol-gel method, then heat-treated at $400^{\circ}C\;and\;800^{\circ}C$ in air atmosphere. The condition of heat treatment was determined by thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTA). The characterization of the lithium manganese oxide was done by X-ray diffraction (XRD) spectra and scanning electron microscopy (SEM). The electrochemical characteristics of lithium manganese oxide electrode for lithium ion battery were measured by cyclic voltammetry (CV), chronoamperometry and AC impedance method using constant charge/discharge process. The electrochemical behaviors of the electrode have been investigated in a 1.0M $LiClO_4/propylene$ carbonate electrolyte solution. The diffusivity of lithium ions, $D^+\;_{Li}\;^+$, as determined by AC impedance technique was $6.2\times10^{-10}cm^2s^{-1}$.
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