• Title/Summary/Keyword: Residue analysis

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Analysis of Residual Fluoroquinolones Contents in Fish (어류 중 Fluoroquinolone계 항균제의 분석 및 잔류량 조사)

  • Park, Young-Ae;Yuk, Dong-Hyun;Kim, Su-Un;Kim, Jin-Ah;Park, Ae-Sook;Kim, Youn-Cheon;Kim, Moo-Sang
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.293-299
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    • 2012
  • The residual contents of fluoroquinolones in fish and shrimp were analyzed by using HPLC-FLD and LC-MS. The limit of detection (LOD) and limit of quantification (LOQ) for fluoroquinolones by HPLC-FLD were 0.0030-0.0083 and 0.0090-0.0252 mg/kg, respectively. Those by LC-MS were 0.0019-0.0040 and 0.0059-0.0122 mg/kg, respectively. Recoveries regarding ofloxacin, norfloxacin, pefloxacin, ciprofloxacin and enrofloxacin ranged from 76.4-104.6%. The detection rate of fluoroquinolones was 7.5% from a total of 268 samples. In only one Korean bullhead sample, the sum of ciprofloxacin and enrofloxacin contents was detected at a higher level than its maximum residue limits (MRL) of 0.1 mg/kg. Ofloxacin, norfloxacin and pefloxacin were not detected in any samples and detection rates of ciprofloxacin and enrofloxacin were 3.4% and 6.7%, respectively. In detection rate by species eel (2.6%), loach (2.2%), Korean bullhead (1.5%), carp (0.7%) and snakehead (0.4%) were in order.

Accurate determination of chloramphenicol in meat by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS) (동위원소희석 액체크로마토그래피-질량분석법을 이용한 육류 중 클로람페니콜의 정밀한 정량 분석에 관한 연구)

  • Song, Hye-Min;Kim, Byung-Joo;Jeong, Hyuk;Ahn, Seong-Hee
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.524-530
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    • 2010
  • Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

A Study on the Content of Heavy Metals of Marine Fish in Korean Coastal water (우리나라 일부연안 해산 어류 중의 중금속 함량에 관한 연구)

  • 성덕화;이용욱
    • Journal of Food Hygiene and Safety
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    • v.8 no.4
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    • pp.231-240
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    • 1993
  • This study was carried out to find out the content of injurious heavy metals, such as mercury, lead, cadmium and arsenic of marine fish which had been captured in adjacent sea of Korea. From March, 1 to April, 30 in 1993. 60 sample of fishes were collected the adult fish and young fish. These samples were analyzed by the Mercury Analyzer and Inductively Coupled Plasma Emission Spectro Analyzer. The results of the study were summarized as follows: (1) The content of mercury in Therafra chalcograma was 0.112$\pm$0.034 ppm which was higher than other fishes, but Pseudosciaena manchurica and Pampus argenteus had lower (P<0.05). Although lead content of Trichiurus lepturus was 0.359$\pm$0.056 ppm, which was higher than other fishes. The lead content of Theragra chalcograma had lower to the almost same level. The cadmium content of the Theragra chalcograma was 0.069$\pm$0.010 ppm which was higher than other samples, but Pseudosciaena manchurica had 0.039$\pm$0.020 ppm to lower level. Though there was some fluctuation in the arsenic content which was 0.433~3.752 ppm, the arsenic content of Therafra chalcograma was 3.752$\pm$2.873 ppm which was the higher than any other fishes. But there are not statistical significances. (2) Heavy metal content by the maturity of the fishes: Mercury content of the old Pseudosciaena manchurica was 0.055$\pm$0.15 ppm comparing to the young's result of 0.030$\pm$0.009 ppm (P<0.05). Though there were some differences according to the maturity, but thee was no statistical significance. (3) In view of the correlation of the heavy metal content, for Pseudosciaena manchurica, high correlation was founded to r=0.6437 between mercury and cadmium (P<0.05). Though the content of mercury, arsenic cadmium and lead had positive correlation (r=0.2725) and negative correlation (r=-0.3958), but there was no significance at all. The other fishes were not found correlation between the heavy metal content. Positive correlation was found between age with mercury in Pseudociaena manchurica (r=0.7018, P<0.05). The negative correlation of age with lead content in the Pseudociaena Manchurica was signigicant (P<0.05). The correlation coefficient was r=-0.7623. The age with mercury content in Coloabis saira had high correlation (r=0.7201, P<0.05). Through the above analysis, it can get conclusion that injurious heavy metal content of the fishes in Korea such a mercury, lead, cadmium and arsenic were at the level of natural content. At present, guidelines of maximum residue level allowed at foreign countries about the injurious heavy metal have been used according to the kinds of fish but our government guideline for the marine fishes in only total mercury below 0.7 ppm and lead below 2 ppm. So more aggressive guidelines for the allowance level of heavy metals in marine fishes are required for the safety of foods.

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Studies on Analytical Methods for N-Methylcarbamate Residues in Crops by Spectrophotometry and Gas Liquid Chromatography (작물체중(作物體中) N-Methylcarbamate계(系) 농약(農藥)의 잔류분석법(殘留分析法)에 관(關)한 연구(硏究))

  • Oh, Byung-Youl;Jeong, Young-Ho;Park, Young-Sun
    • Korean Journal of Environmental Agriculture
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    • v.1 no.1
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    • pp.14-21
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    • 1982
  • Analytical methods for residues of six N-methylcarbamate insecticides were investigated to compare the minimum detectability, recovery from several crops and feasibility of multiple residue analysis. Those methods studied in this work included spectrophotometry by diazotization and gas chromatography by N-trifluoroacetylation(TFA), pentafluorobenzylether(PFB) and dinitrophenylether (DNP) derivatization. Maximum absorbed wavelength of the diazotized MIPC, XMC, BPMC, propoxur and carbofu ran was around 460 ㎚, while that of carbaryl recorded 510 ㎚. Recovery from brown rice and apple by diazotization method ranged from 80 to 120% and minimum detectable limits were 0.03 to 0.05 ppm in 50 g of the sample. Minimum detectability of PFB derivatives by gas chromatography was superior to TFA and DNP derivatives. DNP derivatives showed the longest retention time among the given derivatives. Recovery from crops by gas chromatographic met hod ranged 74 to 94%, 78 to 93%, and 85 to 99% in brown rice, rice straw and apple, respectively. Limit of detection was 0.01 ppm for TFA, 0.005 ppm for PFB and 0.02 ppm for DNP derivatives in 50 g of the crop samples.

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Effects of Calcium Chloride Concentration and Reaction Time on Physical and Sensory Characteristics of Persimmon Calcium Alginate Beads (염화칼슘 농도와 반응시간에 따른 감 칼슘 알지네이트 비드의 물리적 및 관능적 특성)

  • Yong, Dong-Hee;Song, Min-Kyung;Yoon, Hye-Hyun
    • Culinary science and hospitality research
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    • v.18 no.4
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    • pp.209-221
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    • 2012
  • The purpose of this study is to apply molecular gastronomy and its spherification methodology to persimmon desserts. We prepared persimmon calcium alginate beads and investigated physical and sensory characteristics of beads according to the different concentration of calcium chloride(0.5, 0.75, 1.0%) and reaction time(2, 4, 6, 8, 10 min). Lightness and yellowness were decreased significantly as both calcium chloride concentration and reaction time increased. However, redness was increased significantly as the concentration of calcium chloride and reaction time increased. Hardness, springiness, chewiness, cohesiveness, and resilience except for adhesiveness tended to increase as the concentration of calcium chloride and reaction time increased. The thickness of beads also increased as the concentration of calcium chloride and reaction time increased. Quantitative descriptive analysis showed that voluminosity, springiness, hardness, chewiness, and residue tended to increase as the concentration of calcium chloride increased. Overall acceptability reached a peak at the persimmon bead containing 0.5% calcium chloride. The result of this study showed that the concentration of calcium chloride and reaction time influenced the overall characteristics of calcium alginate beads.

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Crystal Structure and Thermal Stability Study on Tetrabutylammonium Hexamolybdate [n-Bu4N]2[Mo6O19](TBAM)

  • Zhao, Pu Su;Zhao, Zhan Ru;Jian, Fang Fang;Lu, Lu De
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.553-558
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    • 2003
  • The crystal structure of $[n-Bu_4N]_2[Mo_6O_{19}]$(TBAM) (n-Bu4N=tetrabutylammonium) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters ${\alpha}$=16.314(5), b=17.288(5), c=17.776(4)${\AA}$ ${\beta}$=101.47(3), and Z=4. In $[Mo_6O{19}]^{2-}$ anion, Mo atoms occupy six vertices of octahedron and each Mo atom is coordinated by six oxygen atoms to adopt distorted octahedral coordination geometry. The average bond distance of Mo-Ot (terminal), Mo-Ob (bridged) and Mo-Oc (central) are 1.680 ${\AA}$, 1.931 ${\AA}$ and 2.325 ${\AA}$ respectively. In $[n-Bu_4N]^+$ cation, the N atom possesses a slightly distorted tetrahedral geometry. There are some potential extensive C-H ${\cdots}$ O hydrogen bonds in the lattice, by which connecte molecules and stabilize the crystal structure. Thermogravimetric analysis suggests that thermal decomposition of the title compound includes two transitions and it loses weight at 356.0 and 803.5 $^{\circ}$, respectively, and the residue presumable be $Mo_2O_2$. Accordingly, the title compound has high thermal stability.

Congener Specific Profiles and Exposure Pathways of Polybrominated Diphenyl Ethers (PBDEs) in Breast Milk of Chuncheon Area (춘천지역 모유 중 폴리브롬화디페닐메테르(PBDEs)의 이성체별 분포특성과 노출경로)

  • We, Sung-Ug;Baek, In-Cheon;Park, Sang-Ah;Kang, Seong-Hoon;Cho, Yu-Jin;Cho, Bong-Hui;Yoon, Cho-Hee;Kim, Ki-Ho;Min, Byung-Yoon
    • Journal of Life Science
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    • v.20 no.3
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    • pp.356-364
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    • 2010
  • This study was carried out to investigate the exposure pathway of PBDEs in human breast milk collected from new mothers residing in Chuncheon, a comparatively clean area in Korea. The congeners of PBDE in 22 human breast milk samples were analyzed using a high resolution gas chromatography with a high resolution mass detector. The residue level of ${\sum}PBDEs$ was higher in primipara subjects than in multipara subjects (p<0.05). The levels in this study were similar to those of people in some Asian and European countries, but were lower than those of people in north America. In the congener profiles, BDE-47 (mean contribution=36.1%) was predominant, followed by BDE-153 (27%), BDE-99 (11.7%), BDE-100 (11.1%), BDE-28 (7.9%) and BDE-183 (3.5%). The sum of BDE-47 and BDE-153 accounted for more than 50% of ${\sum}PBDEs$ in most samples. BDE-47 was highly correlated with ${\sum}PBDEs$ (r=0.94, p<0.001). No strong trend was observed between PBDE levels and a number of key biological factors (women's age, weight, height and body mass index) examined in this study, however, weak correlations were observed in PBDE levels measured against dietary habits, particularly in fish consumption frequency. It seems that Korean people might be exposed to multiple sources including products of PBDEs, and particularly food resources.

Characteristics of Microwave Leaching for the Removal of Bi, As from the Sulfide Mineral Concentrate (황화광물정광으로부터 Bi, As 제거를 위한 마이크로웨이브 용출 특성)

  • On, Hyun-Sung;Togtokhmaa, B.;Park, Cheon-Young
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.3
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    • pp.137-147
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    • 2018
  • The aim of this study was to leach penalty elements, such as Bi and As, effectively through microwave leaching of a gold concentrate sample containing penalty elements with nitric acid solution. For this purpose, the time effect of microwave leaching, nitric acid concentration effect, and sample addition effect in a microwave were examined. The experiment, demonstrated that the leaching rate of penalty elements increased as microwave leaching time and nitric acid concentration increased and concentration addition decreased. When a microwave heating experiment was carried out on the concentrate and ore minerals, Bi was removed by as much as 90%, and the phase of arsenopyrite was transformed in the order of arsenopyrite (FeAsS), pyrrhotite (FeS), and hematite ($Fe_2O_3$). When the X-ray diffraction (XRD) analysis was carried out with solid residue, elemental sulfur and anglesite were identified. The intensity of the XRD peaks of elemental sulfur and anglesite increased, and the peaks were sharper when the microwave leaching time was 12 min instead of 1 min, the nitric acid concentration was 4 M in rather than 0.5 M, and the concentration addition was 30 g rather than 5 g. This was probably because more elemental sulfur and anglesite were generated in the leaching solution as the leaching efficiency increased. Bi can be leached as valuable elements in the leaching solution through microwave leaching processes while they are released to the environment through a microwave heating processes.

Establishment of analytical method of methiozolin and dissipation in golf course's green (Methiozolin의 분석법 개발 및 골프장 그린에서의 잔류소실특성)

  • Jo, Hyeong-Wook;Hwang, Kyu-won;Hwang, Ki-Hwan;Moon, Joon-Kwan
    • Journal of Applied Biological Chemistry
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    • v.59 no.4
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    • pp.331-336
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    • 2016
  • Analytical methods for methiozolin in soil, water and turfgrass were established and dissipation patterns of methiozolin in soil and turfgrass were elucidated. Analysis was done using a high performance liquid chromatography with an ultra violet detector at the wavelength of 280 nm after extraction with acetone, liquid-liquid partition with dichloromethane, and a solid phase extraction purification. Limit of determination and Limit of quantitation were 1.0, 0.5, 1.0 ng, and 0.001, 0.1, 0.01 mg/kg for water, turfgrass, and soil, respectively. Recovery rates of methiozolin from soil, water, and turfgrass were ranged 87.5~111.3, 92.8~97.4, and 78.2~98.5 %, respectively. The turfgrass and soil samples were collected at 0, 1, 4, 7, 14, 30, 45, and 60 after spray on green area in golf course. Residues of methiozlolin were not translocated to lower soil layer but detected only in turfgrasses and root area of turfgrass. Half-lives of methiozolin in turfgrass were 10.7 days and 8.8 days in soil from root area.

A study on the denitrification and microbial community characteristics by the change of C/N ratio of molasses and nitrate nitrogen (당밀과 질산성 질소의 C/N ratio 변화에 따른 탈질 및 미생물 군집 특성에 관한 연구)

  • Eom, Hanki;Kim, Sungchul
    • Korean Journal of Microbiology
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    • v.54 no.2
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    • pp.105-112
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    • 2018
  • To compare the denitrification efficiency, this study used molasses and methanol were used as external carbon sources. Specific experimental conditions were classified according to C/N ratio conditions. The batch test showed that the denitrification efficiency increased as C/N ratios of molasses and methanol rose. The most suitable C/N ratio of molasses turned out 4:1 considering the concentration of the residue chemical oxygen demand (COD) and the denitrification efficiency, which was 91.4%. Specific denitrification rate (SDNR) drawn as a kinetic factor demonstrated that molasses and methanol showed similar SDNR values as C/N ratios of molasses and methanol increased. Under the condition of C/N ratio 4:1, 0.0292 g $NO_3{^-}-N$ removal/g mixed liquor volatile suspended solid (MLVSS)/day (molasses), 0.0299 g $NO_3{^-}-N$ removal/g MLVSS/day (methanol) were found. Sludge adapted to molasses showed that Bacterium Pseudomonas sp. and Bergeylla sp. dominated through an analysis of microbial community. In addition, some bacteria were high convergences than the variety of microbial community. Accordingly, it was assumed that molasses focus on growing microorganisms specialized in denitrification and applied as a replaceable external carbon source that can enhance denitrification performance.