• Title/Summary/Keyword: 0.1N HCl

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Development of LC-MS/MS Quantitation Method for Ethoxyquin in Fishery Products (수산물 중 에톡시퀸의 LC-MS/MS 정량분석법 개발)

  • Shin, Dasom;Chae, Young-Sik;Kang, Hui-Seung;Lee, Soo-Bin;Cho, Yoon-Jae;Cheon, So-Young;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.6
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    • pp.432-438
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    • 2016
  • Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

Protective Effects of HEAC and its Primary Active Compound on HCl-ethanol Induced Gastritis in Rats (흰쥐에서 염산-에탄올로 유발된 위염에 대한 HEAC 추출물과 그 주성분의 억제효과)

  • Choi, Won-Sik;Jang, Do-Yoen;Lee, Gyung-Rak;Kim, Seung-Han
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.13 no.4
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    • pp.1769-1776
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    • 2012
  • The purpose of this study is to evaluate the gastric mucosal damage effect by Hericium erinaceus cultibated with Artemisia capillaris (HEAC) with 0.15 M HCl in ethanol in rats. Among them, 80% ethanol extract showed potent inhibitory effect (67.7%) on gastritis. Using solvent fractionation, 80% ethanol extract of HEAC was separated into five fractions with $n$-hexane, methylene chloride, ethyl acetate, $n$-butanol and water. As a result, fractions obtained with methylene chloride exhibited strong inhibitory effects on gastritis. With this result, the methylene chloride extract was analyzed by GC/MS, HPLC, IR and NMR($^1H$, $^{13}C$) to identify primary active components and the main component in the extract was identified as ethyl linoleate. The effective does ($ED_{50}$) values of 80% ethanol extract of HEAC and ethyl linoleate showed 22.6 and 6.4 mg/kg, respectively and these values were higher than those of stillen (44.2 mg/kg) and selbex (46.5 mg/kg). Therefore, the administration of 80% ethanol extract of HEAC and ethyl linoleate have a strong protective effect agasint the gastritis induced by HCl-ethanol and may be promising new drug for treating gastritis and gastric ulcer.

Production of Fine Cobalt Metal Powders from Superalloy Scrap(1) (Treating Superalloy Scrap with Zinc) (Superalloy 스크랩으로부터 Co 미분말의 제조(1) (Superalloy 스크랩의 아연처리))

  • 박문경;이영근
    • Resources Recycling
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    • v.4 no.1
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    • pp.52-59
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    • 1995
  • Treating bulk superalloy scrap with molten zinc has been studled to facililate recycling and recovery- of cobalt.Superalloys investigated were the cobalt-base Mar-M-509 and X45 and the nickel-base Rene 80. Charges withZnlscrap ratlos of 1.5-6.5 were heated to 750-9002 far 1-7.5 hours in a nitrogen atmosphere. The moltenzinc dissolved superalloy scrap and zinc was removed by vacuum distillation at 850-Wk for 4-6 hours. Ithas been concluded that the optimum conditions of decomposition for Mar-M-509 and Rene 80 \"ere dissolutiontemperature of about 850k, Znlscrap ratlo of about 5, and dissalution time of about 5.5 hours. The zinc-treatedsuperalloy prouducts were friable and reacted rapidly with acid solutions. Leaching 9mm pieces of unalloyedMar-M-509 or Rene 80 with 5 times the stolchlometric amount oi 6N HCI at 90t ior 3 hours dissolved about1.5-7.270, while leachmg of the minus 20-mesh products dissolved about 89.0-93.0%.ved about 89.0-93.0%.

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Addition Effects of Alkali Metal Oxide on Some Properties of Porous Glass-Ceramics in the $CaO-TiO_2-P_2O_5$ System ($CaO-TiO_2-P_2O_5$계 다공질 결정화 유리의 물성에 미치는 알카리 금속 산화물의 첨가효과)

  • 장순규;최세영
    • Journal of the Korean Ceramic Society
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    • v.31 no.11
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    • pp.1337-1345
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    • 1994
  • Glasses in the system of 45CaO-25TiO2-30P2O5 containing 1 mole% of M2O(M=Li, Na, K) were melted and crystallized. And their crystal phases were Ca3(PO4)2, CaTi4(PO4)6, and TiO2. Porous glass-ceramics with skeleton of two crystal phase CaTi4(PO4)6 and TiO2 were prepared by selective leaching of Ca3(PO4)2 with 0.1 N-HCl. Glass transition temperature(Tg) and crystallization temperature(Tc) were decreased by addition of 1 mole% alkali metal oxide. Pore size of porous glass-ceramics was increased with increasing heat treatment temperature and its dependence on heat treatment temperature was decreased with addition of Na2O and K2O. It was found that porous glass-ceramics of parent glass and containing 1mole% M2O(M=Li, Na, K) composition had maximum specific surface area, porosity and maximum of crystallzed phase by heat treatment at 80$0^{\circ}C$, 76$0^{\circ}C$, 78$0^{\circ}C$, 80$0^{\circ}C$ respectively.

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Determination of Ketorolac in Human Serum by High-performance Liquid Chromatography

  • Chun, In-Koo;Kang, Hyun-Hee;Gwak, Hye-Sun
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.529-534
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    • 1996
  • A high-performance liquid chromatographic (HPLC) assay has been developed for the determination of ketorolac in human serum using a new extraction method with a good recovery. Human serum samples (1.0 ml) spiked with known concentrations of ketorolac tromethamine and 10${\mu}g$ of ketoprofen as the internal standard (IS) were acidified with 200${\mu}l$ of 1 N HCl and extracted with 7 ml of n-hexane-ether (7:3 v/v). Extracts were centrifuged and organic layer was back-extracted with 400${\mu}l$ of 0.1% tromethamine solution. Twenty .mu.l of centrifuged aqueous layer was injected onto a reversed-phase octyl column and eluted with a mixture of acetonitrile, water, methanol, and triethylamine [35:55:10:0.1 (v/v), pH 3.0] at a flow rate of 1.0 ml/min. Ultraviolet detection of ketorolac and IS was carried out at 300 nm. The calibration curve obtained using peak area ratios showed a good linearity (in concentration range 10-150 ng/ml $r^2$=O.9944; in range 50-2000 ng/ml, r$^{2}$=0.9998). The mean intra-day accuracy and precision for this HPLC method were found to be 3.6 and 3.7%, respectively. The mean inter-day accuracy and precision were found to be 4.0 and 3.7%, respectively, in the concentration range 50-2000 ng/ml. The recovery of ketorolac from serum was 92.0 $({\pm}5.7)$ % at the concentration of 100 ng/ml. This method proved to be readily applicable to the assay of ketorolac in human serum.

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Effect of Salts and Temperature upon the Rate and Extent of Aggregation of Casein during Acidification of Milk (산에 의한 우유단백질의 응고속도에 염과 온도가 미치는 영향)

  • Kim, Byung-Yong;Kim, Myung-Hwan;Kinsella, John E.
    • Korean Journal of Food Science and Technology
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    • v.24 no.1
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    • pp.42-48
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    • 1992
  • The rate and extent of coagulation of milk using fast acidification with 0.1 N HCl were monitored by changes in viscosity and turbidity at various temperatures and pH. Also the gelation rate of milk using slow acidification with D-glucono-${\delta}$-lactone was measured in a small strain rheological scanner. Coagulation of milk casein occurred in a specific pH range and was accompanied by an abrupt increase in viscosity at pH 5.0. Acid coagulation rate was enhanced by increasing temperature from $20^{\circ}C{\sim}50^{\circ}C$, and the maximum rate was shown around pH 5.0. The addition of salt ($CaCl_{2}$) reduced the maximum coagulation rate at all temperature ranges and shifted the pH ranges for maximum coagulation rate and the onset pH of coagulation. The onset of gelation and the rate of network formation during slow acidification were facilitated by Cl ion, but suppressed by SCN-ion, as indicated by the rate of rigidity development. The susceptibility to syneresis was greater in the gel made at lower temperature and around pH 4.6, while preheated milk at $90^{\circ}C$ for 5 min prior to acidification showed the same syneresis profile at all heating temperatures ($60{\sim}90^{\circ}C$).

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Freshness of 'Fuji' Apples Packed MA Film Treated with Acid and Anti-fogging Agents (산 및 결로방지 처리한 기능성 MA포장으로 포장한 '후지' 사과의 신선도)

  • Park, Hyung-Woo;Ryu, Na-Hee
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.19 no.1
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    • pp.43-50
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    • 2013
  • This study investigated the effect of functional MA films (FMA) masterbatched by zeolite powder treated with 1 N HCl solution and anti-fogging agent (CA) on the freshness extension of 'Fuji' Apples. Preference, weight loss, total ascorbic acid, sugar content, acidity, change of gas composition in package were evaluated during storage at $15^{\circ}C$. After 150 days of storage, the weight loss of LLDPE film (control, L) apples was 0.4%, and that of apple in FMA film (CA) was 1.1%. Total ascorbic acid content of apples in control after 150 days was 2.09 mg%, and those of apple in FMA film was 2.94 mg%. The titratable acidity of apple in FMA film was higher than that in control, while soluble solids content of packages was lower than that in control after 150 days. Ethylene gas adsorbability in control package was 192.2 ppm and those in FMA film was 165.6 ppm. Overall, apples in FMA film was better than that of control. It was verified that apples packed with LLDPE film(control) lasted about 130 days, while those with FMA film lasted about 170 days. Also, FMA film treated with anti-fogging agent achieved no significant effect on freshness extension compared to non-treated film, but quality of 'Fuji' Apples was improved by anti-fogging agent when compared to that of non-treated anti-fogging agent.

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Ammonium Adsorption Property of Acrylic Acid and Styren Grafting Polypropylene Non-Woven Fabric Synthesized by Photo-induced Polymerization (광조사 중합법에 의해 합성된 PP-g-AA와 PP-g-St 부직포의 암모니아성 질소 흡착특성 비교)

  • Park, Hyun-Ju;Na, Choon-Ki
    • Journal of Environmental Science International
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    • v.17 no.11
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    • pp.1255-1263
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    • 2008
  • The efficiency of PP-g-AA and PP-g-St nonwoven fabric synthesized by photoinduced polymerization as an adsorbent for removal $NH_3-N$ from waste water was evaluated. The results evidently indicate that the adsorption capacities of $NH_3-N$ onto PP-g-AA nonwoven fabric were extremely superior to those onto sulfonated PP-g-St nonwoven fabric, PK and zeolite. PP-g-AA nonwoven fabric showed the maximum adsorption capacity of $NH_3-N$ at the degree of grafting of 80 wt.%. The adsorption behaviour of $NH_3-N$ onto PP-g-AA and sulfonated PP-g-St nonwoven fabric was controlled by an ion exchange reaction, and tended to be similar to both trends of Langmiur and Freundlish isotherm. Futhermore, PP-g-AA non-woven fabric could be regenerated more than 5 times by a simple washing with 0.1N HCl with no decrease of adsorption capacity and no degradation of physical properties. Also sulfonated PP-g-St nonwoven fabric could be regenerated by washing with 0.1N ${H_2}{O_4}$. However, their regeneration efficiency was significantly low because grafting layer acted as functional radical for adsorption was continuously desquamated in the adsorption or regeneration processes, which resulted in decrease of adsorption capacity and weight of adsorbent. All results obtained from this study indicate that the $NH_3-N$ removal capacity of PP-g-AA non-woven fabric was extremely superior to those of PP-g-St non-woven fabric, PK and zeolite.

Synthesis, Characterization and DNA Interaction Studies of (N,N'-Bis(5-phenylazosalicylaldehyde)-ethylenediamine) Cobalt(II) Complex

  • Sohrabi, Nasrin;Rasouli, Nahid;Kamkar, Mehdi
    • Bulletin of the Korean Chemical Society
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    • v.35 no.8
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    • pp.2523-2528
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    • 2014
  • In the present study, at first, azo Schiff base ligand of (N,N'-bis(5-phenylazosalicylaldehyde)-ethylenediamine) ($H_2L$) has been synthesized by condensation reaction of 5-phenylazosalicylaldehyde and ethylenediamine in 2:1 molar ratio, respectively. Then, its cobalt complex (CoL) was synthesized by reaction of $Co(OAc)_2{\cdot}4H_2O$ with ligand ($H_2L$) in 1:1 molar ratio in ethanol solvent. This ligand and its cobalt complex containing azo functional groups were characterized using elemental analysis, $^1H$-NMR, UV-vis and IR spectroscopies. Subsequently, the interaction between native calf thymus deoxyribonucleic acid (ct-DNA) and CoL complex was investigated in 10 mM Tris/HCl buffer solution, pH = 7 using UV-vis absorption, thermal denaturation technique and viscosity measurements. From spectrophotometric titration experiments, the binding constant of CoL complex with ct-DNA was found to be $(2.4{\pm}0.2){\times}10^4M^{-1}$. The thermodynamic parameters were calculated by van't Hoff equation.The enthalpy and entropy changes were $5753.94{\pm}172.66kcal/mol$ and $43.93{\pm}1.18cal/mol{\cdot}K$ at $25^{\circ}C$, respectively. Thermal denaturation experiments represent the increasing of melting temperature of ct-DNA (about $0.93^{\circ}C$) due to binding of CoL complex. The results indicate that the process is entropy-driven and suggest that hydrophobic interactions are the main driving force for the complex formation.

Physicochemical properties of chitosans produced from shrimp shell under the different conditions and their influences on the properties of Kakdugi during storage (제조조건이 다른 새우껍질 chitosan의 물리.화학적 성질 및 깍두기의 보존성에 미치는 영향)

  • Kim, Kwang-Ok;Kang, Hyen-Jun
    • Journal of the Korean Society of Food Culture
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    • v.9 no.1
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    • pp.71-77
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    • 1994
  • This study was undertaken to investigate the physicochemical properties of chitosans produced from chitins which were prepared from shrimp shell under the 4 different conditions(HCl concentration : 1 N, 4 N and reaction temperature $0^{\circ}C,\;20^{\circ}C$). The effects of chitosan on the properties of Kakdugi during storage also were examined. Viscosity of chitosan was markedly different$(313.1{\sim}98.8\;cps)$ depending on the production conditon. Chitosan solution showed pseudoplastic property. The infrared(IR) spectrums of chitosans prepared under the conditions of this study were very simillar, and the degree of deacetylation of chitosan was relatively high$(92{\sim}96%)$ independent of the extraction conditions of chitin. As the storage period was extended, markedly lower pH and higher titratable acidity were resulted in all the groups. Throughout the storage period, pH and titratable acidity of kakdugies with chitosan were higher and lower, respectively than those of control. Viscosity of kakdugi juice was significantly different among the groups and as the storage period increased, the juice viscosity decreased. At the eighth day of storage, the juice of control group was more viscous than those of kakdugies containing chitosan. Throughout the storage period the numbers of total microorganisms and of microorgarnisms of Leuconostoc genus in control kakdugi tended to be higher and lower, respectively than those in kakdugies containing chitosan. The growth of Lac. plantarum was slightly lower in kakdugi containing chitosan C produced at low HCl concentration and high temperature compared to the others.

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