• Title/Summary/Keyword: matrix solid phase dispersion

Search Result 26, Processing Time 0.022 seconds

Comparison of pretreatment methods for tetracyclines analysis by HPLC (테트라싸이클린계 잔류항생물질 분석을 위한 전처리방법 비교)

  • Kim, Dong-Eon;Hwang, Lae-Hwong;Yun, En-Sun;Ham, Hee-Jin;Yang, Yoon-Mo;Kim, Chang-Gi;Ki, No-Jun;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
    • /
    • v.26 no.3
    • /
    • pp.199-202
    • /
    • 2003
  • Solid phase extraction(SPE) and matrix solid phase dispersion(MSPD) have been studied as preparation procedures for tetracyclines analysis by high-performance liquid chromatography(HPLC) in meat. The recovery range was 74${\sim}$98% for SPE, and 72${\sim}$93% for MSPD at spiked levels of 100ng/g for oxytetracycline(OTC), tetracycline(TC), chlortetracycline(CTC), and doxycycline(DC). The detection limits were 15${\sim}$78ng/g for SPE and 25${\sim}$84ng/g for MSPD, respectively. Analytical method was HPLC with UV detector. The purpose of this study was developing a practical, accurate and precise method for rapid extraction and quantitation of tetracycline residues in meat.

Matrix solid phase dispersion isolation and high performance liquid chromatographic determination of five benzimidazole anthelmintics in bovine muscle, liver and omasum (시료고체상분산처리와 액체크로마토그라피를 이용한 소의 근육, 간 및 천엽에서의 벤지미다졸계 구충제 잔류분석)

  • Kim, Chung-Hui;Kim, Gon-Sup;Park, Jung-Hee;Hah, Dae-Sik;Ryu, Jae-Doo;Son, Sung-Gi;Heo, Jung-Ho;Jung, Myung-Ho;Kim, Jong-Shu
    • Korean Journal of Veterinary Research
    • /
    • v.42 no.2
    • /
    • pp.171-181
    • /
    • 2002
  • Simultaneous multiresidue analysis using liquid chromatography determination for five benzimidazole anthelmintics(thiabendazole, oxibendazole, albendazole, mebendazole and fenbendazole) in bovine muscle, liver and omasum has been described. Blank or benzimidazole-fortified samples(0.5g) were blended with bulk $C_{18}$($40{\mu}m$, 18% load, endcapped, 2g). A column made from the resultant $C_{18}$/animal tissue matrix was first washed with hexane($8m{\ell}$), following which the benzimidazoles were eluted with acetonitrile($8m{\ell}$). Analytes of extracted sample were determined by liquid chromatography with UV detector at 290nm. Correlation coefficients of standard curves for individual benzimidazole isolated from fortified samples, using internal standardization, were linear($0.991{\pm}0.007$ to $0.996{\pm}0.005$) with average relative percentage recoveries from $62.1{\pm}3.8(%)$ to $92.3{\pm}7.5(%)$ for the concentration range($0.2{\sim}6.4{\mu}g/g$), respectively. Recoveries rates of TBZ, MBZ in liver, OBZ, MBZ in muscle and TBZ, MBZ in omasium from fortified benzimidazole were 92.%, 87.3%, 74.5%, 82.7%, 75.2% and 83.5% at condition II, respectively. Condition II showed higher recoveries rates than condition I. These results indicated that the matrix solid phase dispersion(MSPD) methodology is acceptable for the determination of 5 benzimidazole anthelmintics and may also suitable for other matrixes of food animal origin.

Multiresidue matrix solid phase dispersion (MSPD) extraction and HPLC determination of tetracyclines in animal muscle tissue (시료고체상분산(matrix solid phase dispersion)전처리법을 이용한 식육중 테트라사이클린계 항생물질 동시정량분석)

  • Kang, Hwan-goo;Son, Seong-wan;Cho, Byung-hoon;Lee, Hye-sook;Park, Shin-ja;Kim, Jae-hak;Cho, Myung-haing
    • Korean Journal of Veterinary Research
    • /
    • v.36 no.3
    • /
    • pp.541-550
    • /
    • 1996
  • Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{\sim}1.0{\mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{\circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{\mu}g/g$ for OTC and TC, and $0.1{\mu}g/g$ for CTC and DC.

  • PDF

Microstructure and Characteristics of Mechanically Alloyed Ni-W(WC) (기계적 합금화한 Ni-W(WC)의 미세구조 및 특성)

  • Sin, Su-Cheol;Jang, Geon-Ik
    • Korean Journal of Materials Research
    • /
    • v.8 no.12
    • /
    • pp.1133-1137
    • /
    • 1998
  • By the mechanical alloying method Ni-W(WC) composite materials were prepared to improve the resistance for creep and sintering of Ni-anode at the operating temperature of$ 650^{\circ}C$. Amorphization was observed from the XRD analysis of mechanically alloyed powder caused by the destruction of ordered crystals. Sintering was performed at $1280^{\circ}C$ for 10 hours in $H_2$ atmosphere. From the result of dot-mapping and TEM analysis the second phase was not observed at Ni-W interface while W particles of less 0.lam were distributed finely and uniformly in Ni matrix. This finely and uniformly distributed W in Ni matrix is expected to enhance the mechanical properties of Ni-anode through the dispersion and solid solution hardening mechanisms.

  • PDF

Study on the development of simultaneous-rapid screening methods for residues pesticides in livestock products (수입 축산식품에서의 잔류농약 동시분석법 개발에 관한 연구)

  • Kim, Jong-shu;Kim, Gon-sup;Hah, Dae-sik
    • Korean Journal of Veterinary Research
    • /
    • v.37 no.1
    • /
    • pp.213-220
    • /
    • 1997
  • A simple and rapid method known as matrix solid phase dispersion(MSPD) for simultaneous determination of 11 pesticide(2,4,5,6-tetrachlor m-xylene, ${\alpha}$-BHC, ${\gamma}$-BHC, ${\delta}$-BHC, aldrin, chlorfulazuron, heptachloroepoxide, dieldrine, endrin, endosulfan sulfate, and tetradifon) in beef fat was estabilished. Beef fat(0.5g) was fortified by adding the 11 pesticides and dibutylchlorendate as internal standard, and blended with 2g bulk $C_{18}$ in pestle and motar. Pesticides were eluted from an extraction column composed of $C_{18}$/ fat matrix blend and 2g activated Florisil by addition of 8ml acetonitrile. Then $2{\mu}l$ portion of the acetonitrile elute was directly analyzed by gaschromatography with electron capture detection. Unfortified blank control were treated similarly. Recovery rate were ranged from $83{\pm}5.4%$ to $94.2{\pm}7.6%$, intra-assay variability and inter-assay variability were ranged from 2.3% to 7.4%(n=5 for each insecticides) and from $6{\pm}1%$ to $12{\pm}3%$(n=10 for each insecticides), respectively. These results indicated that the MSPD methodology is aceptable for the extraction, determination and screening of residues 11 chroniated pesticides in beef fat.

  • PDF

IRRADIATION PERFORMANCE OF U-Mo MONOLITHIC FUEL

  • Meyer, M.K.;Gan, J.;Jue, J.F.;Keiser, D.D.;Perez, E.;Robinson, A.;Wachs, D.M.;Woolstenhulme, N.;Hofman, G.L.;Kim, Y.S.
    • Nuclear Engineering and Technology
    • /
    • v.46 no.2
    • /
    • pp.169-182
    • /
    • 2014
  • High-performance research reactors require fuel that operates at high specific power to high fission density, but at relatively low temperatures. Research reactor fuels are designed for efficient heat rejection, and are composed of assemblies of thin-plates clad in aluminum alloy. The development of low-enriched fuels to replace high-enriched fuels for these reactors requires a substantially increased uranium density in the fuel to offset the decrease in enrichment. Very few fuel phases have been identified that have the required combination of very-high uranium density and stable fuel behavior at high burnup. U-Mo alloys represent the best known tradeoff in these properties. Testing of aluminum matrix U-Mo aluminum matrix dispersion fuel revealed a pattern of breakaway swelling behavior at intermediate burnup, related to the formation of a molybdenum stabilized high aluminum intermetallic phase that forms during irradiation. In the case of monolithic fuel, this issue was addressed by eliminating, as much as possible, the interfacial area between U-Mo and aluminum. Based on scoping irradiation test data, a fuel plate system composed of solid U-10Mo fuel meat, a zirconium diffusion barrier, and Al6061 cladding was selected for development. Developmental testing of this fuel system indicates that it meets core criteria for fuel qualification, including stable and predictable swelling behavior, mechanical integrity to high burnup, and geometric stability. In addition, the fuel exhibits robust behavior during power-cooling mismatch events under irradiation at high power.

Simultaneous Determination of Tetracyclines and Sulfonamides Residues in Pork and Flatfish Using Matrix Solid Phase Dispersion (MSPD) Extraction and HPLC (MSPD와 HPLC를 이용한 돼지고기 및 광어 중의 테트라싸이클린계 항생제와 sulfonamide의 다성분 잔류분석법 개발)

  • Gil, Geun-Hwan;Ko, Kwang-Yong;Lee, Yong-Jae;Park, Hye-Jin;Lee, Kyu-Seung
    • Korean Journal of Environmental Agriculture
    • /
    • v.28 no.3
    • /
    • pp.266-273
    • /
    • 2009
  • This study was conducted to develop more convenient simultaneous determination method by matrix solid phase dispersion (MSPD) and HPLC for sulfonamides such as sulfamerazine (SMR), sulfamethazine (SMT), sulfamonomethoxine (SMM), sulfadimethoxine (SDM), sulfaquinoxaline (SQX), and tetracyclines including oxytetracycline (OTC), tetracycline (TC) chlortetracycline (CTC) in prok and flatfish. The limits of detection were 0.047 $mg{\cdot}kg^{-1}$ for OTC, TC, SMR, SMT and SMM, and 0.033 $mg{\cdot}kg^{-1}$ for CTC, SDM, and SQX, respectively. So it is sufficiently possible to detect the eight tetracyclines and sulfonamides under their MRLs ($0.1{\sim}0.2mg{\cdot}kg^{-1}$). The average percentage recoveries of sulfonamides and tetracyclines from pig muscle and flatfish spiked standard solution were approximately $80.25{\sim}101.25%$ and $85.77{\sim}121.42%$, respectively. Therefore this method was efficient for simultaneous analysis of eight tetracyclines and sulfonamides.

Sheet fabrication of Ni-WC anode for Molten Carbonate Fuel Cell by Tape Casting Method (테이프 캐스팅법에 의한 MCFC Anode용 Ni-WC 박판 제조)

  • Choe, Jin-Yeong;Jeong, Seong-Hoe;Jang, Geon-Ik
    • Korean Journal of Materials Research
    • /
    • v.10 no.10
    • /
    • pp.715-720
    • /
    • 2000
  • By the mechanical alloying method. Ni-WC composite materials were prepared to improve the deformation-resistance for creep and sintering of Ni-anode at the operating temperature of $650^{\circ}C$. Mechanically alloyed powder w was initially fabricated by ball milling for 80hr, and then amorphization was occurred by the destruction of ordered crystals based on XRD analysis. In order to investigate the electrochemical performance and sheet characteristics of Ni-WC anode, tape casting process was adopted. Finally, the obtained sheet thickness of Ni- we after sintering at $1180^{\circ}C$ for 60 minutes in $H_2$ atmosphere was O.9mm and the average pore size was $3~5{\mu\textrm{m}}$ with porosities of 55%. The second phase was not observed in Ni- W matrix while W particles were finely and uniformly distributed in Ni matrix. This fine and uniform distributed W particles in Ni matrix are expected to enhance the mechanical properties of Ni anode through the dispersion and solid solution hardening mechanisms.

  • PDF

Thermal Compatibility of High Density U-Mo Powder Fuels Prepared by Centrifugal Atomization

  • Kim, Ki-Hwan;Ahn, Hyun-Suk;Chang, Se-Jung;Ko, Young-Mo;Lee, Don-Bae;Kim, Chang-Kyu;Kuk, Il-Hyun
    • Proceedings of the Korean Nuclear Society Conference
    • /
    • 1997.05b
    • /
    • pp.165-170
    • /
    • 1997
  • Samples of extruded dispersions of 24 vol.% spherical U-2wt%Mo and U-10wt.%Mo powders in an aluminum matrix were annealed for over 2,000 hours at 40$0^{\circ}C$. No significant dimensional changes occurred in the U-1025.%Mo/aluminum dispersions. The U-2wt.%Mo/aluminum dispersion, however, increased in volume by 26% after 2,000 hours at 40$0^{\circ}C$. This large volume change is mainly due to the formation of voids and cracks resulting from nearly complete interdiffusion of U-Mo and aluminum. Interdiffusion between U-10wt.%Mo and aluminum was found to be minimal. The different diffusion behavior is primarily due to the fact that U-2wt.%Mo decomposes from an as-atomized metastable r-phase(bcc) solid solution into the equilibrium r-U and U$_2$Mo two-phase structure during the experiment, whereas U-10wt.%Mo retains the metastable r-phase structure after the 2,000 hours anneal and thereby displays superior thermal compatibility with aluminum compared to U-2wt.%Mo. In addition, the molybdenium supersaturated in U-10wt.%Mo particles inhibits the diffusion of aluminum atoms along the grain boundary into the particle. Also, the dissolution of only a few Mo atoms in UAL$_3$ retards the formation of the intermediate phase, as Mo atoms need to migrate from new intermetallic compounds to unreacted islands.

  • PDF

Simultaneous Quantification of Sulfonamide and Tetracyclines in Fish Muscle Tissue by Matrix Solid Phase Dispersion (MSPD) Extraction and HPLC (MSPD와 HPLC를 이용한 어류의 잔류 설파제와 테트라사이클린계 항생물질의 동시분석)

  • 하대식;김종수;김곤섭
    • Journal of Food Hygiene and Safety
    • /
    • v.12 no.2
    • /
    • pp.117-124
    • /
    • 1997
  • A simple, rapid and simultaneous analytical method is described for the detection of Sulfonamide and Tetracycline residues, i.e., Sulfamerazine (SMR), Sulfamethazine (SMT), Sulfamonomethoxine (SMM), Sulfadimethoxine (SDM), Sulfaquinoxaline (SQN), Oxytetracycline (OXY), Tetracycline (TC), Chlortetracycline (CTC). Blank control and sulfonamide and tetracycline fortified fish muscle samples (0.5 f) were blended with octadecylsilyl (C18, 40 ${\mu}{\textrm}{m}$, 21% load, 60$\AA$) derivatized silica packing material (2 g). Blended fish samples were washed with hexane, then, benzene and dichloromethace were used for the elution of tetracycline and sulfonamide were analyzed by HPLC. Correlation coefficients of standard curves for individual sulfonamide and tetracycline isolated from fortified samples were linear (0.9993$\pm$0.0003~0.9997$\pm$0.0003, 0.9493$\pm$0.078~0.9753$\pm$0.036), respectively. The average percentage recoveries of sulfonamide and tetracycline ranged as 80.86~96.52% to 85.88~92.23%, and 30.01~37.12% to 65.89~73.40%, for the concentration range (0.1~1.0 ppm) examined, respectively. Limit of detection for sulfonamide was 0.0012 ppm for SMR in Paralichthys Olivacleus and 0.0020 ppm for SMR, 0.015 ppm for SMM in Cyprinus Carpio. The applicability of this procedure is demonstrated by separation and detection of incurred tetracycline and sulfonamide residues in fish muscle tissue.

  • PDF