• Title/Summary/Keyword: Solution stability

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Preparation and Keeping Quality of Vacuum Packed Seasoned-Dried Sardine (진공포장 정어리 조미건제품의 제조 및 품질안정성)

  • LEE Eung-Ho;KIM Jin-Soo;KIM Han-Ho;LEE Jin-Kyung;OH Kwang-Soo;KWON Chil-Sung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.19 no.1
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    • pp.52-59
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    • 1986
  • As one of trials to process instant sardine foods which can be preserved at room temperature, three kinds of products were prepared as seasoned-dried product (control, C), liquid smoked seasoned-dried product(S) and antioxidant treated seasoned-dried product(E), and their processing conditions and quality stability during storage were examined. Raw sardines were dressed, steamed and then filleted. The sardine fillets were seasoned with the mixed seasoning solution containing $28.0\%$ of sorbitol, $14.0%$ of sugar, $5.6\%$ of table salt, $1.8\%$ of monosodium glutamate, $0.6\%$ of garlic powder and $50.0\%$ of water at $5^{\circ}C$ for 15 hours, and dipped for 45 seconds in $10\%$ Smoke-EZ solution. After liquid smoking, the seasoned and liquid smoked sardine fillets were dried at $45^{\circ}C$ for 4 hours, vacuum packed in laminated plastic film bag(polyester/casted polypropylene= $12{\mu}m/70{\mu}m,\;15{\times}16cm$), and finally pasteurized in water at $95^{\circ}C$ for 30 minutes. The results obtained from chemical and microbial experiments during storage are as follows : the moisture contents, water activity and pH of the products showed little change, and VBN of them slightly increased during storage. The TBA value and POV of the products (E, S) were lower than those of control product(C) considerably. In color values, L value (linghtness) decreased while a and b value (red and yellow) revealed a tendency to increase during storage. The fatty acid composition of the products were similar to those of raw sardine, the predominant fatty acids were 16:0, 20:5, 18:1 and 22:6. The products (E, S) have a good preservative effect on highly unsturated fatty acids during storage. Viable cell counts of those products were negative and histamine contents were less than 2.0 mg/100 g. Among the texture profiles, hardness, elasticity and cohesiveness of the products slightly decreased during storage. Judging from the sensory evaluations, liquid smoked seasoned-dried product(S) was the most desirable, and the products could be preserved in good condition for 40 days at $25{\pm}3^{\circ}C$.

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Studies on In situ and In vitro Degadabilities, Microbial Growth and Gas Production of Rice, Barley and Corn (쌀, 보리, 옥수수의 반추위내 In situ 및 In vitro 분해율, 미생물 성장과 Gas 발생량에 대한 연구)

  • 이상민;강태원;이신자;옥지운;문여황;이성실
    • Journal of Animal Science and Technology
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    • v.48 no.5
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    • pp.699-708
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    • 2006
  • Ground rice, barley and corn were fed separately to the ruminally cannulated Hanwoo (Korean native cattle) for comparing their in situ and in vitro degradabilities, microbial growth, pH and gas production. It has been found that nearly all the dry matter (DM) and organic matter (OM) in barley and rice disappeared during 24 hr suspension in the rumen, but those in corn were only reduced by around 67%. Water soluble DM and OM fractions(‘a’), ranked from highest to lowest was corn, then rice and finally barley, but the order was reversed for content ‘b’, degradable fraction during time ‘t’. Judging by the degradation parameter of ‘b’ fraction, degradation rates per hour of DM and OM for barley were 38.3% and 37.2% respectively, significantly higher than those for rice (7.7% and 5.6%) and corn (4.1% and 1.3%). In general, results obtained from in vitro degradability of DM and OM were lower than those from in situ trials, but the ranking order of degradability was in agreement between both trials. In particular, ground rice has relatively lower in vitro microbial growth than corn or barley, but exhibited higher gas production. In addition, in vitro microbial growth of ground rice increased with up to 12 hr of incubation period, thereafter experienced a decrease with extended incubation time. pH of in vitro solution of rice decreased following 9 hr of incubation but gas production increased rapidly during the same period. From the results of DM and OM degradabilities and pH changes of in vitro solution with incubation time, it is concluded that rice represents a good source of energy for stability of rumen fermentation.

Swelling and Mechanical Property Change of Shale and Sandstone in Supercritical CO2 (초임계 CO2에 의한 셰일 및 사암의 물성변화 및 스웰링에 관한 연구)

  • Choi, Chae-Soon;Song, Jae-Joon
    • Tunnel and Underground Space
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    • v.22 no.4
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    • pp.266-275
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    • 2012
  • In this study, a method is devised to implement a supercritical $CO_2$ ($scCO_2$) injection environment on a laboratory scale and to investigate the effects of $scCO_2$ on the properties of rock specimens. Specimens of shale and sandstone normally constituting the cap rock and reservoir rock, respectively, were kept in a laboratory reactor chamber with $scCO_2$ for two weeks. From this stage, a chemical reaction between rock surface and the $scCO_2$ was induced. The effect of saline water was also investigated by comparing three conditions ($scCO_2$-rock, $scCO_2-H_2O$-rock and $scCO_2$-brine(1M)-rock). Finally, we checked the changes in the properties before and after the reaction by destructive and nondestructive testing procedures. The swelling of shale was a main concern in this case. The experimental results suggested that $scCO_2$ has a greater effect on the swelling of the shale than pure water and brine. It was also observed that the largest swelling displacement of shale occurred after a reaction with the $H_2O-scCO_2$ solution. The results of a series of the destructive and nondestructive tests indicate that although each of the property changes of the rock differed depending on the reaction conditions, the $H_2O-scCO_2$ solution had the greatest effect. In this study, shale was highly sensitive to the reaction conditions. These results provide fundamental information pertaining to the stability of $CO_2$ storage sites due to physical and chemical reactions between the rocks in these sites and $scCO_2$.

People's heart-and-mind and the righteous principle in the hostile of circumstances / focusing on Yeheon's Record of Taking Refuge (난중(亂中)의 인심(人心)과 의리(義理) - 여헌(旅軒) 장현광(張顯光)의 『용사일기(龍蛇日記)』를 중심으로 -)

  • Jeon, Byoung-Ok
    • (The)Study of the Eastern Classic
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    • no.57
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    • pp.9-40
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    • 2014
  • This article focuses on Yeheon's consideration and solution for the hostile of social circumstances during the time of the Japanese invasions. Yeheon thought that the Chosun dynasty must have faced such disorder before the war happened. People including the king and his subjects did not live their life according to the righteous principle, and the state was not under control in a way that it should accomplish the Dao. Yeheon thought that the Japanese invasion, which is more like a flood or certain disasters, was not primarily responsible for the harshest of environments. Yeheon paid his attention to the fact that even after the Japanese invasions ended, people were still in disorder losing their mind-and-heart. People's mind-and-heart became that of animals because of starvation and disease. This is because the government made people trapped in a difficult situation by forcing them to prepare for military operations, rather than taking care of them. As a result, in Yeheon's view, the main cause of the social disorder was people's lack of mind-and-heart, which brought about their actions of brutality like those of animals. Although Yeheon himself did not form righteous armies, he instead suggested a right path to overcome and solve the social disorder by describing and analyzing in detail the reality of the war as well as the problems of policies. In particular, Yeheon studied the Zhou yi at the time because understanding the principle of fortune and misfortune, as well as the rise and fall of a state, could give a proper solution to the social turmoil of his times. In Yeheon's eyes, the most important thing to do in the time of people's losing mind-and-heart was to follow li and accomplish the Dao in their daily life. And this was what he, as a gentleman, should do. Yeheon thought that in spite of the harshest of environments, one can still preserve one's grace and dignity, which would overcome one's adversity. This gives us the following questions: should one put aside one's grace and dignity to overcome wartime perils? Or in so doing, one should face more severe time after a short period of peace and stability? These questions concern the relationship between one's morality and the state's responsibility, and what is the right way of doing one's duty to the state is the main philosophical subject in this article.

Counter-Piracy Cooperation to Strengthen New Southern Policy's "Peace": An Analysis of ROK and ASEAN's Counter-Piracy Practices (신남방정책의 "평화"를 강화하기 위한 해적행위 대응 협력: 한국과 아세안의 해적행위 대응 관행 분석)

  • Boo, Yerin;Kim, Sujin;Yeo, Mathew Jie Sheng
    • Maritime Security
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    • v.3 no.1
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    • pp.141-185
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    • 2021
  • The growing U.S.-China rivalry has placed the countries of Southeast Asia in exceedingly precarious positions. The Republic of Korea (ROK) likewise has been tasked with the challenge of "navigating the waters" between deepening geopolitical divides. It is in this context that the "New Southern Policy" (hereafter NSP) has become a key word in Korea's foreign policy circles. Through NSP, ROK aims to diversify its economic and security interests by strengthening ties with its southern partners, focusing on three key areas (termed as the "3 Ps"): People, Prosperity, and Peace. At the same time, the NSP seeks cooperation with other key diplomatic agendas such as the U.S.'s "Free and Open Indo-Pacific," rendering it crucial for the overall stability of the region. Considering such strategic significance, deeper analysis of the policy is more timely than ever. A brief assessment of the policy's outcome so far, however, reveals that relatively, the "Peace" pillar has been insufficient in achieving satisfactory outcomes. Here, this paper asks the question of: 1) How can the "Peace" pillar of South Korea's New Southern Policy be strengthened? Based on an analysis on the causes of the "Peace" pillar's weakness, this paper identifies counter-piracy cooperation as a solution. This paper then proceeds to answer the next question of: 2) How can ROK and ASEAN cooperate on counter-piracy, and how can these efforts be integrated into ROK's NSP? To answer the above question, this paper conducts in-depth case studies on ASEAN's and ROK's approaches to counter-piracy and identifies specific mechanisms of cooperation. In Chapter I, the paper begins with an overview of the NSP's strategic significance and an evaluation of its "Peace" pillar. Chapter II conducts a literature review on the causes of, and prescriptions for, the weakness of the "Peace" pillar. The paper then justifies why counter-piracy may be a solution. Chapter III examines ASEAN's and ROK's approaches to counter-piracy. By analyzing the general framework and each region's cases, the paper displays the strengths and weaknesses of each region's piracy responses. Based on this analysis, Chapter IV suggests ways to incorporate counter-piracy cooperation into the "Peace" pillar of the NSP. This research bears significance in that it identifies a specific area of cooperation (counter-piracy) to strengthen the "Peace" pillar of ROK's NSP. Such identification is based on a comprehensive study into the two parties' past and current experience in counter-piracy, making it contextual in nature. Furthermore, the study suggests practical mechanisms of cooperation, and considers ways of incorporation into the existing framework of NSP. This approach differs from existing literature that failed to generate case-specific, policy-oriented solutions. The COVID-19 pandemic has exacerbated piracy issues and deepened geopolitical divides. Turbulent seas such as these call for careful navigation. When it comes to promoting "peace," the key lies in combating the pirates that sail those very waters.

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Effects on the Rumen Microbial Fermentation Characteristics of Lignosulfonate Treated Soybean Meal (Lignosulfonate처리 대두박의 반추위 내 미생물 발효특성에 미치는 영향)

  • Lee, Hun-Jong;Lee, Seung-Heon;Bae, Gui-Seck;Park, Je-Hwan;Chang, Moon-Baek
    • Journal of Animal Science and Technology
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    • v.52 no.5
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    • pp.413-426
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    • 2010
  • This study was conducted to investigate the effects on fermentation characteristics of rumen microorganism by different types and levels of lignosulfonate treated soybean meal (LSBM) in in vitro test and rumen simulation continuous culture (RSCC) system in dairy cows. The experiment I was control and 12 treatments (each with 3 replications) in vitro test to demonstrate composition of different types of treatments with lignosulfonate (Desulfonate, Na, Ca and solution) and levels (2, 4 and 8%) of soybean meal in the dairy cow diet. LSBM source treatments in the dairy cow diet showed pH value, $NH_3$-N concentration and total VFA concentration lower than control at all levels and incubation times (p<0.05). Dry matter digestibility of LSBM source treatments showed lower than control (p<0.05). Gas production and rumen microbial synthesis was decreased by rumen microbial fermentation for incubation times. Undegradable protein (UDP) concentration of all LSBM treatments was decreased for incubation times, and significantly higher than control (p<0.05). In the experiment II compared diets of the control, LSBM Na 2%, LSBM Sol 2%, which are high performance to undegradable protein (UDP) concentration experiment I in vitro test, and heated treatment lignosulfonate (LSBM Heat) 2% in the dairy cow diet from four station RSCC system ($4{\times}4$ Latin square). A rumen microbial fermentation characteristic was stability during 12~15 days of experimental period in all treatments. The pH value of LSBM treatments was higher than control treatment (p<0.05). The $NH_3$-N concentration, VFA concentration and rumen microbial synthesis of LSBM treatments were lower than control (p<0.05). The undegradable protein (UDP) showed LSBM Na 2% (45.28%), LSBM Sol 2% (43.52%) and LSBM Heat 2% (43.49%) higher than control (41.55%), respectively (p<0.05). Those experiments were designed to improve by-pass protein of diet and milk protein in the dairy cows. We will conduct those experiments the in vivo test by LSBM treatments in dairy cows diet.

Pharmacological Studies of Cefoperazone(T-1551) (Cefoperazone(T-1551)의 약리학적 연구)

  • Lim J.K.;Hong S.A.;Park C.W.;Kim M.S.;Suh Y.H.;Shin S.G.;Kim Y.S.;Kim H.W.;Lee J.S.;Chang K.C.;Lee S.K.;Chang K.C.;Kim I.S.
    • The Korean Journal of Pharmacology
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    • v.16 no.2 s.27
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    • pp.55-70
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    • 1980
  • The pharmacological and microbiological studies of Cefoperazone (T-1551, Toyama Chemical Co., Japan) were conducted in vitro and in vivo. The studies included stability and physicochemical characteristics, antimicrobial activity, animal and human pharmacokinetics, animal pharmacodynamics and safety evaluation of Cefoperazone sodium for injection. 1) Stability and physicochemical characteristics. Sodium salt of cefoperazone for injection had a general appearance of white crystalline powder which contained 0.5% water, and of which melting point was $187.2^{\circ}C$. The pH's of 10% and 25% aqueous solutions were 5.03 ana 5.16 at $25^{\circ}C$. The preparations of cefoperazone did not contain any pyrogenic substances and did not liberate histamine in cats. The drug was highly compatible with common infusion solutions including 5% Dextrose solution and no significant potency decrease was observed in 5 hours after mixing. Powdered cefoperazone sodium contained in hermetically sealed and ligt-shielded container was highly stable at $4^circ}C{\sim}37^{\circ}C$ for 12 weeks. When stored at $4^{\circ}C$ the potency was retained almost completely for up to one year. 2) Antimicrobial activity against clinical isolates. Among the 230 clinical isolates included, Salmonella typhi was the most susceptible to cefoperazone, with 100% inhibition at MIC of ${\leq}0.5{\mu}g/ml$. Cefoperazone was also highly active against Streptococcus pyogenes(group A), Kletsiella pneumoniae, Staphylococcus aureus and Shigella flexneri, with 100% inhibition at $16{\mu}g/ml$ or less. More than 80% of Escherichia coli, Enterobacter aerogenes and Salmonella paratyphi was inhibited at ${\leq}16{\mu}/ml$, while Enterobacter cloaceae, Serratia marcescens and Pseudomonas aerogenosa were somewhat less sensitive to cefoperagone, with inhibitions of 60%, 55% and 35% respectively at the same MIC. 3) Animal pharmacokinetics Serum concentration, organ distritution and excretion of cefoperazone in rats were observed after single intramuscular injections at doses of 20 mg/kg and 50 mg/kg. The extent of protein binding to human plasma protein was also measured in vitro br equilibrium dialysis method. The mean Peak serum concentrations of $7.4{\mu}g/ml$ and $16.4{\mu}/ml$ were obtained at 30 min. after administration of cefoperazone at doses of 20 mg/kg and 50 mg/kg respectively. The tissue concentrations of cefoperazone measured at 30 and 60 min. were highest in kidney. And the concentrations of the drug in kidney, liver and small intestine were much higher than in blood. Urinary and fecal excretion over 24 hours after injetcion ranged form 12.5% to 15.0% in urine and from 19.6% to 25.0% in feces, indicating that the gastrointestinal system is more important than renal system for the excretion of cefoperazone. The extent of binding to human plasma protein measured by equilibrium dialysis was $76.3%{\sim}76.9%$, which was somewhat lower than the others utilizing centrifugal ultrafiltration method. 4) Animal pharmacodynamics Central nervous system : Effects of cefoperazone on the spontaneous movement and general behavioral patterns of rats, the pentobarbital sleeping time in mice and the body temperature in rabbits were observed. Single intraperitoneal injections at doses of $500{\sim}2,000mg/kg$ in rats did not affect the spontaneous movement ana the general behavioral patterns of the animal. Doses of $125{\sim}500mg/kg$ of cefoperazone injected intraperitonealy in mice neither increased nor decreased the pentobarbital-induced sleeping time. In rabbits the normal body temperature was maintained following the single intravenous injections of $125{\sim}2,000mg/kg$ dose. Respiratory and circulatory system: Respiration rate, blood pressure, heart rate and ECG of anesthetized rabbits were monitored for 3 hours following single intravenous injections of cefoperazone at doses of $125{\sim}2,000mg/kg$. The respiration rate decreased by $3{\sim}l7%$ at all the doses of cefoperazone administered. Blood pressure did not show any changes but slight decrease from 130/113 to 125/107 by the highest dose(2,000 mg/kg) injected in this experiment. The dosages of 1,000 and 2,000 mg/kg seemed to slightly decrease the heart rate, but it was not significantly different from the normal control. All the doses of cefoperazone injected were not associated with any abnormal changes in ECG findings throughout the monitering period. Autonomic nervous system and smooth muscle: Effects of cefoperazone on the automatic movement of rabbit isolated small intestine, large intestine, stomach and uterus were observed in vitro. The autonomic movement and tonus of intestinal smooth muscle increased at dose of $40{\mu}g/ml$ in small intestine and at 0.4 mg/ml in large intestine. However, in stomach and uterine smooth muscle the autonomic movement was slightly increased by the much higher doses of 5-10 mg/ml. Blood: In vitro osmotic fragility of rabbit RBC suspension was not affected by cefoperazone of $1{\sim}10mg/ml$. Doses of 7.5 and 10 mg/ml were associated with 11.8% and 15.3% prolongation of whole blood coagulation time. Liver and kidney function: When measured at 3 hours after single intravenous injections of cefoperaonze in rabbits, the values of serum GOT, GPT, Bilirubin, TTT, BUN and creatine were not significantly different from the normal control. 5) Safety evaluation Acute toxicity: The acute toxicity of cefoperazone was studied following intraperitoneal and intravenous injections to mice(A strain, 4 week old) and rats(Sprague-Dawler, 6 week old). The LD_(50)'s of intraperitonealy injected cefoperazone were 9.7g/kg in male mice, 9.6g/kg in female mice and over 15g/kg in both male and female rats. And when administered intravenously in rats, LD_(50)'s were 5.1g/kg in male and 5.0g/kg in female. Administrations of the high doses of the drug were associated with slight inhibition of spontaneous movement and convulsion. Atdominal transudate and intestinal hyperemia were observed in animals administered intraperitonealy. In rats receiving high doses of the drug intravenously rhinorrhea and pulmonary congestion and edema were also observed. Renal proximal tubular epithelial degeneration was found in animals dosing in high concentrations of cefoperazone. Subacute toxicity: Rats(Sprague-Dawley, 6 week old) dosing 0.5, 1.0 and 2.0 g/kg/day of cefoperazone intraperitonealy were observed for one month and sacrificed at 24 hours after the last dose. In animals with a high dose, slight inhibition of spontaneous movement was observed during the experimental period. Soft stool or diarrhea appeared at first or second week of the administration in rats receiving 2.0g/kg. Daily food consumption and weekly weight gain were similar to control during the administration. Urinalysis, blood chemistry and hematology after one month administration were not different from control either. Cecal enlargement, which is an expected effect of broad spectrum antibiotic altering the normal intestinal microbial flora, was observed. Intestinal or peritoneal congestion and peritonitis were found. These findings seemed to be attributed to the local irritation following prolonged intraperitoneal injections of hypertonic and acidic cefoperazone solution. Among the histopathologic findings renal proximal tubular epithelial degeneration was characteristic in rats receiving 1 and 2g/kg/day, which were 10 and 20 times higher than the maximal clinical dose (100 mg/kg) of the drug. 6) Human pharmacokinetics Serum concentrations and urinary excretion were determined following a single intravenous injection of 1g cefoperazone in eight healthy, male volunteers. Mean serum concentrations of 89.3, 61.3, 26.6, 12.3, 2.3, and $1.8{\mu}g/ml$ occured at 1,2,4,6,8 and 12 hours after injection respectively, and the biological half-life was 108 minutes. Urinary excretion over 24 hours after injection was up to 43.5% of administered dose.

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Determination of Optimal Concentration of LPE (Lysophosphatidylethanolamine) for Postharvest Stability and Quality of Strawberry Fruit (딸기 수확 후 저장기간 연장 및 품질 개선을 위한 LPE (Lysophosphatidylethanolamine) 적정 처리농도 구명)

  • Choi, Ki-Young;Kim, Il-Seop;Yun, Young-Sik;Choi, Eun-Young
    • Journal of Bio-Environment Control
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    • v.25 no.3
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    • pp.153-161
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    • 2016
  • This study aims to determine the optimal maturity of strawberry fruits as affected by the application of lysophosphatidylethanolamine (LPE) and its optimal concentration for postharvest stability and quality. Prior to application of treatments, fruits that were classified into levels of maturity (0%, 50%, 70% and 100%) were air-dried for 40 minutes and stored in the refrigerator at $4^{\circ}C$ for 12 days. Fruits at 70% maturity were dipped into 0, 10, 50 and $100mg{\cdot}L^{-1}$ LPE solutions for 1 minute. A lower range of concentration (0, 2.5, 5, 10 and $25mg{\cdot}L^{-1}$) was applied to fruits at different maturity levels. Data on fresh weight, hardness at vertical and horizontal loading positions, color index and sugar content during storage were collected. Based on fruits with 70% maturity dipped in LPE concentrations, there were no significant differences found on fresh weight, color index and sugar content. However, the application of $10mg{\cdot}L^{-1}$ LPE gave the highest hardness at vertical loading position while $100mg{\cdot}L^{-1}$ had the lowest average. At lower range of LPE concentrations, fresh weight was not significantly affected by LPE application and maturity levels. Hardness of fruits was mainly based on the maturity of the fruits. Increased hardness was observed in the fruits with 70% maturity dipped into the $5mg{\cdot}L^{-1}$ of LPE solution. The hardness and Hunter's $L^*$ and $b^*$ value of 100% matured fruits gave lowest values despite the application of $25mg{\cdot}L^{-1}$ LPE 12 days after storage.

Transition Metal Dichalcogenide Nanocatalyst for Solar-Driven Photoelectrochemical Water Splitting (전이금속 디칼코제나이드 나노촉매를 이용한 태양광 흡수 광화학적 물분해 연구)

  • Yoo, Jisun;Cha, Eunhee;Park, Jeunghee;Lim, Soo A
    • Journal of the Korean Electrochemical Society
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    • v.23 no.2
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    • pp.25-38
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    • 2020
  • Photoelectrochemical water splitting has been considered as the most promising technology for generating hydrogen energy. Transition metal dichalcogenide (TMD) compounds have currently attracted tremendous attention due to their outstanding ability towards the catalytic water-splitting hydrogen evolution reaction (HER). Herein, we report the synthesis method of various transition metal dichalcogenide including MoS2, MoSe2, WS2, and WSe2 nanosheets as excellent catalysts for solar-driven photoelectrochemical (PEC) hydrogen evolution. Photocathodes were fabricated by growing the nanosheets directly onto Si nanowire (NW) arrays, with a thickness of 20 nm. The metal ion layers were formed by soaking the metal chloride ethanol solution and subsequent sulfurization or selenization produced the transition metal chalcogenide. They all exhibit excellent PEC performance in 0.5 M H2SO4; the photocurrent reaches to 20 mA cm-2 (at 0 V vs. RHE) and the onset potential is 0.2 V under AM1.5 condition. The quantum efficiency of hydrogen generation is avg. 90%. The stability of MoS2 and MoSe2 is 90% for 3h, which is higher than that (80%) of WS2 and WSe2. Detailed structure analysis using X-ray photoelectron spectroscopy for before/after HER reveals that the Si-WS2 and Si-WSe2 experience more oxidation of Si NWs than Si-MoS2 and Si-MoSe2. This can be explained by the less protection of Si NW surface by their flake shape morphology. The high catalytic activity of TMDs should be the main cause of this enhanced PEC performance, promising efficient water-splitting Si-based PEC cells.

Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.161-170
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    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.