A rapid analytical method based on capillary electrophoresis is described for the determination of trace anions in high-purity chemicals which is used to prevent corrosion demage in nuclear power plants. Separations are carried out at 20kV using trimethylsilane-coated fused-silica capillary ($70cm{\times}50$ or $75{\mu}m$ i.d.) with the electrolyte of 5mM Chromate(pH=8). Detection was achieved using on-column indirect photometry at 254nm. The simultaneous analysis of inorganic anions, chloride, nitrate, sulfate, azide and phosphate was performed using methods of hydrodynamic(>1ppm) and / or electrokinetic(<1ppm) injection. The results of studies on the coexisting anions on analyte ions shows that peak responses of analyte in hydrodynamic injection is constant without effect of coexisting anions, but those of analysis in electrokinetic injection is strongly dependant upon the kind of coexisting anions and its ionic mobility. The analyte enrichment rate, hence peak response, is positive relationship with the resistance of the sample solution. Thus, appropriate measures, such as standard addition or internal standard technique, must be used to account for differences in conductance of standard and sample solutions.
MMP-1 inhibitory compounds were isolated from 120 Korean traditional edible plants. UP- 1 activity significantly increased linearly with increasing UVB dose in normal human foreskin fibroblast HS68 cell, showing maximum activity at approximately 35 $mJ/cm^2$, whereas in HaCaT cell, normal human keratinocyte, no increase was observed. Maximum secretion of MMP-1 after UVB treatment occurred around 36-48 k after treatment. MMP-1 inhibitory compound isolated from cold-water fraction of Cataegus pinnatifida Bunge showed the mort potent activity. The MMP-1 inhibitory compound was deduced as a peptide based on the fact that pronase digestion decreased the activity whereas periodate oxidation did not. The most potent UP- 1-inhibitory protein, CP-2Va-2, showing an activity of 88.5% against MMP-1, was isolated through sequential column chromatography on DEAE-Toyopearl 650C, Butyl-Toyopearl 650M, and Bio-Gel P-30. Molecular weight of CP-2Va-2 determined through high performance liquid chromatography and SDS PACE was 19 and 20 kDa. respectively, signifying a monomeric structure.
Kim, Jai-Hyun;Paik, Young-Ki;Kim, Jong-Bum;Kim, Jong-Guk;Hwang, Young-Soo;Ha, Sun-Hwa
Applied Biological Chemistry
/
v.41
no.1
/
pp.47-52
/
1998
3-Hydroxy-3-methylglutaryl-CoA reductase (HMGR) catalyzes the conversion of HMG-CoA to mevalonic acid, the first intermediate of isoprenoid biosynthetic pathway in plants. The enzyme was solubilized with 0.4% Brij (polyoxyethylene ether) W-1 from a microsomal fraction of etiolated rice seedlings (Oryza sativa L.) in which its maximal activity was observed on the fourth day after germination. HMGR was purified to near homogeneity by employing $(NH_4)_2SO_4$ fractionation plus chromatographic procedures including DEAE-Sephadex A-50 and HMG-CoA-hexane-agarose affinity column. The size of the purified enzyme was estimated to be 55 kDa when judged by SDS-PAGE analysis with silver staining method. The apparent $K_m$ and $V_{max}$ values for HMG-CoA were determined to be $180\;{\mu}M$ and 107 pmol/min/mg, and those for NADPH were $810\;{\mu}M$ and 32.1 pmol/min/mg, respectively.
A rapid, simple and sensitive LC/MS/MS method for the determination of lercanidipine in human serum was validated and applied to the pharmacokinetic study of lercanidipine. Lercanidipine and internal standard, amlodipine, were extracted from human serum by liquid-liquid extraction with hexan-isoamyl alcohol (100: 1, v/v) and analyzed on a $Symmetry^{(R)}$ MS $C_{18}$ column with the mobile phase of acetonitrile-0.2% aqueous formic acid (70: 30, v/v). Using MS/MS with multiple reaction monitoring (MRM) mode, lercanidipine and amlodipine were detected without severe interferences from human serum matrix. Lercanidipine produced a protonated precursor ion ($[M+H]^+$) at m/z 612.3 and a corresponding product ion at m/z 280.0. Internal standard produced a protonated precursor ion ($[M+H]^+$]) at m/z 409.0 and a corresponding product ion at m/z 238.0. The ruggedness of this method was investigated using quality control (QC) samples. This method showed linear response over the concentration range of 0.05-20 ng/mL with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 mL of serum was 0.05 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the developed method ranged from 85.51 to 112.2% for lercanidipine with overall precision (% C.V.) being 3.56-13.1%. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of lercanidipine in human serum samples for the pharmacokinetic studies, demonstrating the suitability of the method.
Laskar, Arghadeep;Zhong, Jianxia;Mo, Y.L.;Hsu, Thomas T.C.
Interaction and multiscale mechanics
/
v.2
no.1
/
pp.69-89
/
2009
Reinforced and prestressed concrete (RC and PC) thin walls are crucial to the safety and serviceability of structures subjected to shear. The shear strengths of elements in walls depend strongly on the softening of concrete struts in the principal compression direction due to the principal tension in the perpendicular direction. The past three decades have seen a rapid development of knowledge in shear of reinforced concrete structures. Various rational models have been proposed that are based on the smeared-crack concept and can satisfy Navier's three principles of mechanics of materials (i.e., stress equilibrium, strain compatibility and constitutive laws). The Cyclic Softened Membrane Model (CSMM) is one such rational model developed at the University of Houston, which is being efficiently used to predict the behavior of RC/PC structures critical in shear. CSMM for RC has already been implemented into finite element framework of OpenSees (Fenves 2005) to come up with a finite element program called Simulation of Reinforced Concrete Structures (SRCS) (Zhong 2005, Mo et al. 2008). CSMM for PC is being currently implemented into SRCS to make the program applicable to reinforced as well as prestressed concrete. The generalized program is called Simulation of Concrete Structures (SCS). In this paper, the CSMM for RC/PC in material scale is first introduced. Basically, the constitutive relationships of the materials, including uniaxial constitutive relationship of concrete, uniaxial constitutive relationships of reinforcements embedded in concrete and constitutive relationship of concrete in shear, are determined by testing RC/PC full-scale panels in a Universal Panel Tester available at the University of Houston. The formulation in element scale is then derived, including equilibrium and compatibility equations, relationship between biaxial strains and uniaxial strains, material stiffness matrix and RC plane stress element. Finally the formulated results with RC/PC plane stress elements are implemented in structure scale into a finite element program based on the framework of OpenSees to predict the structural behavior of RC/PC thin-walled structures subjected to earthquake-type loading. The accuracy of the multiscale modeling technique is validated by comparing the simulated responses of RC shear walls subjected to reversed cyclic loading and shake table excitations with test data. The response of a post tensioned precast column under reversed cyclic loads has also been simulated to check the accuracy of SCS which is currently under development. This multiscale modeling technique greatly improves the simulation capability of RC thin-walled structures available to researchers and engineers.
A simple and efficient preconcentration method was developed using three-phase liquid phase microextraction prior to HPLC-UV for simultaneous extraction and determination of tetracycline antibiotics (tetracycline, oxytetracycline, and chlortetracycline). The tetracycline antibiotics were separated simultaneously on a column ($C_8$, $3.0{\times}150mm$, $3{\mu}m$) with high selectivity and sensitivity using gradient elution. Under optimized conditions (extraction solvent, heptanal; pH of donor, 9.0; pH of acceptor, 1.0; stirring speed, 700 rpm; NaCl salt, 0%; and extraction time, 60 min), enrichment factors (EF) were between 5.6 and 22.3. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of $0.08{\sim}0.8{\mu}g/mL$ and $0.4{\sim}1.6{\mu}g/mL$, respectively. The calibration curves were linear within the range of $0.1{\sim}32{\mu}g/mL$ with the square of the correlation coefficient being more than 0.995. The precision (as a relative standard deviation, RSD) and accuracy (as a relative recovery) within working range were 1.3~9.1% and 84~118%, respectively.
This study was conducted to understand the source and behavior of organic matter using the fluorescent technique (excitation-emission matrix) as a part of environmental monitoring program in the Korea manganese nodule mining site in the Northeastern Pacific Ocean. Water samples were collected at $0^{\circ},\;6^{\circ}N$, and $10.5^{\circ}N$ along $131.5^{\circ}W$ in August 2005. The concentration of total organic carbon (TOC) ranged from 58.01 to $171.93\;{\mu}M-C$. The vertical distribution of TOC was characterized as higher in the surface layer and decreased with depth. At $6^{\circ}N$, depth-integrated (from surface to 200 m depth) TOC was $337.1\;gC/m^2$, which was 1.4 times higher value than other stations. The exponential decay curve fit of vertical profile of TOC indicated that 59% of organic carbon produced by primary production in the surface layer could be decomposed by bacteria in the water column. Dissolved organic matter is generally classified into two distinctive groups based on their fluorescence characteristics using three-dimensional excitation/emission (Ex/Em) fluorescence mapping technique. One is known as biomacromolecule (BM; protein-like substance; showing max. at Ex 280/Em 330), mainly originated from biological metabolism. The other is geomacromolecule (GM; humic-like substance; showing max. at Ex 330/Em 430), mainly originated from microbial degradation processes. The concentration of BM and GM was from 0.42 to 7.29 TU (tryptophan unit) and from 0.06 to 1.81 QSU (quinine sulfate unit), respectively. The vertical distribution of BM was similar to that of TOC as high in the surface and decreased with depth. However, the vertical distribution of GM showed the reverse pattern of that of BM. From these results, it appeared that BM occupied a major part of TOC and was rapidly consumed by bacteria in the surface layer. GM was mainly transformed from BM by microbial processes and was a dominant component of TOC in the deep-sea layer.
Residual solvents in foods are defined as organic volatile chemicals used or produced in manufacturing of extracts or additives, or functional foods. The solvents are not completely eliminated by practical manufacturing techniques and they also may become contaminated by solvents from packing, transportation or storage in warehouses. Because residual solvents have no nutritional value but may be hazardous to human health, there is a need to remove them from the final products or reduce their amounts to below acceptable levels. The purpose of this study was to develop and evaluate an analytical method for the screening of residual solvents in health functional foods. Furthermore, the aim of this study was to constitute a reasonable management system based on the current state of the market and case studies of foreign countries. Eleven volatile solvents such as MeOH, EtOH, trichloroethylene and hexane were separated depending on their column properties, temp. and time using Gas Chromatography (GC). After determining the GC conditions, a sample preparation method using HSS (Head Space Sampling) was developed. From the results, a method for analyzing residual solvents in health functional foods was developed considering matrix effect and interference from the sample obtained from the solution of solvents-free health functional foods spiked with 11 standards solutions. Validation test using the developed GC/HSS/MS (Mass Spectrometry) method was followed by tests for precision, accuracy, recovery, linearity and adequate sensitivity. Finally, examination of 104 samples grouped in suits was performed by the developed HSS/GC/MS for screening the solvents. The 11 solvents were isolated from health functional foods based on vapor pressure difference, and followed by separation within 15 minutes in a single run. The limt of detection (LOD), limit of quantification (LOQ), recovery and coefficient of variation (C.V.) of these compounds determined by the HSS/GC/MS were found to be 0.1 pg/mL, 0.1-125 pg/g, 51.0-104.6%, and less than 15%, respectively. Using the developed HSS/GC/MS method, residual solvent from 16 out of 104 health functional products were detected as a EtOH. This method therefore seems t o be a valuable extension ofanalytical method for the identification of residual solvents in health functional food.
Choi, Kwang Soon;Kim, Jung Suk;Han, Sun Ho;Park, Soon Dal;Park, Yeong Jae;Joe, Kih Soo;Kim, Won Ho
Analytical Science and Technology
/
v.13
no.5
/
pp.584-591
/
2000
The separation of Nd from the simulated $U_3Si/Al$ spent fuel solution with sequential two-step anion exchange separation has been studied. To prepare the simulated $U_3Si/Al$ spent nuclear fuel, unirradiated $U_3Si/Al$ whose composition consists of small $U_3Si$ particle dispersed in an Al matrix with Al cladding was dissolved with a mixture of 4 M HCl and 10 M $HNO_3$ and 8 or 15 fission product elements were added to the dissolved solution. The trace amount of silica in the solutions was removed by evaporating to dryness with HF and the U was adsorbed on the first anion exchange resin. Neodymium can be purely isolated from the fission product elements with a methanol-nitric acid eluent using the second anion exchange resin. A large excess of Al didn't influence on the elution velocity of Nd, but reduced the eluted contents of Nd, Al, Eu, Gd, Sm and Sr, A large amount of Al was removed first from the column with 3 mL of loading solution (0.8 M $HNO_3$/99.8% MeOH) before Nd elution by the eluent [0.04 M $HNO_3$-99.8% MeOH(1:9)]. The recovery of Nd was more than 94%, regardless of Al contents. Taking the 9 to 13 mL fraction of eluate was effective to purely isolate Nd.
Kim, Jong-Hwan;Kwon, Young Sang;Shin, Min-Chul;Kim, Su Jong;Seo, Jong-Su
Analytical Science and Technology
/
v.29
no.5
/
pp.234-241
/
2016
The approach presented in this article refers to the bioanalytical method validation for the detection and quantitative determination of arsenic species including arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) in dog plasma by high-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP/MS). The arsenic species were separated using an agilent As speciation column by a mobile phase of 2 mM sodium phosphate monobasic, 0.2 mM ethylenediaminetetraacetic acid disodium salt dehydrate, 10 mM sodium acetate, 3 mM sodium nitrate and 1 % ethyl alcohol at pH 11 (adjusted with 1M NaOH). The method validation experiment was obtained selectivity, linearity, accuracy, precision, matrix effect, recovery, system suitability, dilution integrity and various stabilities. All calibration curves showed good linearity (R2>0.999) within test ranges. The lower limit of quantitation (LLOQ) was 5 ng/mL for As(III), As(V) and DMA, and 20 ng/mL for MMA. The system suitability and dilution values were within 6.5 % and 7.7 %. Subsequently, the developed and validated HPLC-ICP/MS method was also successfully applied to determine the arsenic speciation in dog plasma samples, and the recoveries for the spiked samples were in the range of 91.5–102.2 %. Therefore, this method could be applied to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies in biological samples.
본 웹사이트에 게시된 이메일 주소가 전자우편 수집 프로그램이나
그 밖의 기술적 장치를 이용하여 무단으로 수집되는 것을 거부하며,
이를 위반시 정보통신망법에 의해 형사 처벌됨을 유념하시기 바랍니다.
[게시일 2004년 10월 1일]
이용약관
제 1 장 총칙
제 1 조 (목적)
이 이용약관은 KoreaScience 홈페이지(이하 “당 사이트”)에서 제공하는 인터넷 서비스(이하 '서비스')의 가입조건 및 이용에 관한 제반 사항과 기타 필요한 사항을 구체적으로 규정함을 목적으로 합니다.
제 2 조 (용어의 정의)
① "이용자"라 함은 당 사이트에 접속하여 이 약관에 따라 당 사이트가 제공하는 서비스를 받는 회원 및 비회원을
말합니다.
② "회원"이라 함은 서비스를 이용하기 위하여 당 사이트에 개인정보를 제공하여 아이디(ID)와 비밀번호를 부여
받은 자를 말합니다.
③ "회원 아이디(ID)"라 함은 회원의 식별 및 서비스 이용을 위하여 자신이 선정한 문자 및 숫자의 조합을
말합니다.
④ "비밀번호(패스워드)"라 함은 회원이 자신의 비밀보호를 위하여 선정한 문자 및 숫자의 조합을 말합니다.
제 3 조 (이용약관의 효력 및 변경)
① 이 약관은 당 사이트에 게시하거나 기타의 방법으로 회원에게 공지함으로써 효력이 발생합니다.
② 당 사이트는 이 약관을 개정할 경우에 적용일자 및 개정사유를 명시하여 현행 약관과 함께 당 사이트의
초기화면에 그 적용일자 7일 이전부터 적용일자 전일까지 공지합니다. 다만, 회원에게 불리하게 약관내용을
변경하는 경우에는 최소한 30일 이상의 사전 유예기간을 두고 공지합니다. 이 경우 당 사이트는 개정 전
내용과 개정 후 내용을 명확하게 비교하여 이용자가 알기 쉽도록 표시합니다.
제 4 조(약관 외 준칙)
① 이 약관은 당 사이트가 제공하는 서비스에 관한 이용안내와 함께 적용됩니다.
② 이 약관에 명시되지 아니한 사항은 관계법령의 규정이 적용됩니다.
제 2 장 이용계약의 체결
제 5 조 (이용계약의 성립 등)
① 이용계약은 이용고객이 당 사이트가 정한 약관에 「동의합니다」를 선택하고, 당 사이트가 정한
온라인신청양식을 작성하여 서비스 이용을 신청한 후, 당 사이트가 이를 승낙함으로써 성립합니다.
② 제1항의 승낙은 당 사이트가 제공하는 과학기술정보검색, 맞춤정보, 서지정보 등 다른 서비스의 이용승낙을
포함합니다.
제 6 조 (회원가입)
서비스를 이용하고자 하는 고객은 당 사이트에서 정한 회원가입양식에 개인정보를 기재하여 가입을 하여야 합니다.
제 7 조 (개인정보의 보호 및 사용)
당 사이트는 관계법령이 정하는 바에 따라 회원 등록정보를 포함한 회원의 개인정보를 보호하기 위해 노력합니다. 회원 개인정보의 보호 및 사용에 대해서는 관련법령 및 당 사이트의 개인정보 보호정책이 적용됩니다.
제 8 조 (이용 신청의 승낙과 제한)
① 당 사이트는 제6조의 규정에 의한 이용신청고객에 대하여 서비스 이용을 승낙합니다.
② 당 사이트는 아래사항에 해당하는 경우에 대해서 승낙하지 아니 합니다.
- 이용계약 신청서의 내용을 허위로 기재한 경우
- 기타 규정한 제반사항을 위반하며 신청하는 경우
제 9 조 (회원 ID 부여 및 변경 등)
① 당 사이트는 이용고객에 대하여 약관에 정하는 바에 따라 자신이 선정한 회원 ID를 부여합니다.
② 회원 ID는 원칙적으로 변경이 불가하며 부득이한 사유로 인하여 변경 하고자 하는 경우에는 해당 ID를
해지하고 재가입해야 합니다.
③ 기타 회원 개인정보 관리 및 변경 등에 관한 사항은 서비스별 안내에 정하는 바에 의합니다.
제 3 장 계약 당사자의 의무
제 10 조 (KISTI의 의무)
① 당 사이트는 이용고객이 희망한 서비스 제공 개시일에 특별한 사정이 없는 한 서비스를 이용할 수 있도록
하여야 합니다.
② 당 사이트는 개인정보 보호를 위해 보안시스템을 구축하며 개인정보 보호정책을 공시하고 준수합니다.
③ 당 사이트는 회원으로부터 제기되는 의견이나 불만이 정당하다고 객관적으로 인정될 경우에는 적절한 절차를
거쳐 즉시 처리하여야 합니다. 다만, 즉시 처리가 곤란한 경우는 회원에게 그 사유와 처리일정을 통보하여야
합니다.
제 11 조 (회원의 의무)
① 이용자는 회원가입 신청 또는 회원정보 변경 시 실명으로 모든 사항을 사실에 근거하여 작성하여야 하며,
허위 또는 타인의 정보를 등록할 경우 일체의 권리를 주장할 수 없습니다.
② 당 사이트가 관계법령 및 개인정보 보호정책에 의거하여 그 책임을 지는 경우를 제외하고 회원에게 부여된
ID의 비밀번호 관리소홀, 부정사용에 의하여 발생하는 모든 결과에 대한 책임은 회원에게 있습니다.
③ 회원은 당 사이트 및 제 3자의 지적 재산권을 침해해서는 안 됩니다.
제 4 장 서비스의 이용
제 12 조 (서비스 이용 시간)
① 서비스 이용은 당 사이트의 업무상 또는 기술상 특별한 지장이 없는 한 연중무휴, 1일 24시간 운영을
원칙으로 합니다. 단, 당 사이트는 시스템 정기점검, 증설 및 교체를 위해 당 사이트가 정한 날이나 시간에
서비스를 일시 중단할 수 있으며, 예정되어 있는 작업으로 인한 서비스 일시중단은 당 사이트 홈페이지를
통해 사전에 공지합니다.
② 당 사이트는 서비스를 특정범위로 분할하여 각 범위별로 이용가능시간을 별도로 지정할 수 있습니다. 다만
이 경우 그 내용을 공지합니다.
제 13 조 (홈페이지 저작권)
① NDSL에서 제공하는 모든 저작물의 저작권은 원저작자에게 있으며, KISTI는 복제/배포/전송권을 확보하고
있습니다.
② NDSL에서 제공하는 콘텐츠를 상업적 및 기타 영리목적으로 복제/배포/전송할 경우 사전에 KISTI의 허락을
받아야 합니다.
③ NDSL에서 제공하는 콘텐츠를 보도, 비평, 교육, 연구 등을 위하여 정당한 범위 안에서 공정한 관행에
합치되게 인용할 수 있습니다.
④ NDSL에서 제공하는 콘텐츠를 무단 복제, 전송, 배포 기타 저작권법에 위반되는 방법으로 이용할 경우
저작권법 제136조에 따라 5년 이하의 징역 또는 5천만 원 이하의 벌금에 처해질 수 있습니다.
제 14 조 (유료서비스)
① 당 사이트 및 협력기관이 정한 유료서비스(원문복사 등)는 별도로 정해진 바에 따르며, 변경사항은 시행 전에
당 사이트 홈페이지를 통하여 회원에게 공지합니다.
② 유료서비스를 이용하려는 회원은 정해진 요금체계에 따라 요금을 납부해야 합니다.
제 5 장 계약 해지 및 이용 제한
제 15 조 (계약 해지)
회원이 이용계약을 해지하고자 하는 때에는 [가입해지] 메뉴를 이용해 직접 해지해야 합니다.
제 16 조 (서비스 이용제한)
① 당 사이트는 회원이 서비스 이용내용에 있어서 본 약관 제 11조 내용을 위반하거나, 다음 각 호에 해당하는
경우 서비스 이용을 제한할 수 있습니다.
- 2년 이상 서비스를 이용한 적이 없는 경우
- 기타 정상적인 서비스 운영에 방해가 될 경우
② 상기 이용제한 규정에 따라 서비스를 이용하는 회원에게 서비스 이용에 대하여 별도 공지 없이 서비스 이용의
일시정지, 이용계약 해지 할 수 있습니다.
제 17 조 (전자우편주소 수집 금지)
회원은 전자우편주소 추출기 등을 이용하여 전자우편주소를 수집 또는 제3자에게 제공할 수 없습니다.
제 6 장 손해배상 및 기타사항
제 18 조 (손해배상)
당 사이트는 무료로 제공되는 서비스와 관련하여 회원에게 어떠한 손해가 발생하더라도 당 사이트가 고의 또는 과실로 인한 손해발생을 제외하고는 이에 대하여 책임을 부담하지 아니합니다.
제 19 조 (관할 법원)
서비스 이용으로 발생한 분쟁에 대해 소송이 제기되는 경우 민사 소송법상의 관할 법원에 제기합니다.
[부 칙]
1. (시행일) 이 약관은 2016년 9월 5일부터 적용되며, 종전 약관은 본 약관으로 대체되며, 개정된 약관의 적용일 이전 가입자도 개정된 약관의 적용을 받습니다.