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Development and Validation of Analytical Method for Nitroxoline in Chicken Using HPLC-PDA (HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Eun;Kim, Jae-Young;Kang, Ilhyun;Lee, Sang-Mok;Do, Jung-Ah;Oh, Jae-Ho;Chang, Moon-Ik;Hong, Jin-Hwan
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.70-77
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    • 2013
  • BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

Development and validation of an analytical method for fungicide fenpyrazamine determination in agricultural products by HPLC-UVD (HPLC-UVD를 이용한 살균제 fenpyrazamine의 시험법 개발 및 검증)

  • Park, Hyejin;Do, Jung-Ah;Kwon, Ji-Eun;Lee, Ji-Young;Cho, Yoon-Jae;Kim, Heejung;Oh, Jae-Ho;Rhee, Kyu-Sik;Lee, Sang-Jae;Chang, Moon-Ik
    • Analytical Science and Technology
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    • v.27 no.3
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    • pp.172-180
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    • 2014
  • Fenpyrazamine which is a pyrazole fungicide class for controlling gray mold, sclerotinia rot, and Monilinia in grapevines, stone fruit trees, and vegetables has been registered in republic of Korea in 2013 and the maximum residue limits of fenpyrazamine is set to grape, peach, and mandarin as 5.0, 2.0, and 2.0 mg/kg, respectively. Very reliable and sensitive analytical method for determination of fenpyrazamine residues is required for ensuring the food safety in agricultural products. Fenpyrazamine residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica-SPE cartridge and eluted with hexane and acetone mixture. The purified samples were determined by HPLC-UVD and confirmed with LC-MS and quantified using external standard method. Linear range of fenpyrazamine was between $0.1{\sim}5.0{\mu}g/mL$ with the correlation coefficient (r) 0.999. The average recovery ranged from 71.8 to 102.7% at the spiked level of 0.05, 0.5, and 5.0 mg/kg, while the relative standard deviation was between 0.1 and 7.3%. In addition, limit of detection and limit of quantitation were 0.01 and 0.05 mg/L, respectively. The results revealed that the developed and validated analytical method is possible for fenpyrazamine determination in agricultural product samples and will be used as an official analytical method.

Development of an Analytical Method for Fluxapyroxad Determination in Agricultural Commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Fluxapyroxad 잔류분석법 개발)

  • Kwon, Ji-Eun;Kim, HeeJung;Do, Jung-Ah;Park, Hyejin;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.29 no.3
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    • pp.234-240
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    • 2014
  • Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

Physical and cooking characteristic properties of parboiled rice (파보일미(Parboiled rice)의 이화학적 특성 II. 파보일미(추청벼)의 물리적 성질 및 조리특성)

  • 박선희;조은자
    • Korean journal of food and cookery science
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    • v.11 no.2
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    • pp.126-132
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    • 1995
  • This study was undertaken to determine effect of parboiling on physical and cooking characteristic properties of milled rice. Equilibrium moisture content(EMC) of parboiled rice soaked at room tempe-rature(25$^{\circ}C$) and high temperature(75$^{\circ}C$) increased 1.8∼2.7 times & 1.4∼l.6 times as compare to raw rice, and time to reach EMC of parboiled rice became longer 4 times and 1.7 times than raw rice respectively. Equilibrium volume(EV), time to reach EV and volume increase rate constants(ku) were similar to EMC, time to reach EMC, and k. kv of parboiled rice brought about in decrease at room temperature and increase at high temperature. The geletinization temperature, time and peak viscosity of parboiled rice were higher than those of raw rice. Parboiling brought about in decrease in L/W of cooked parboiled rice kernels and L/W increased according to presoaking time was prolo-nged. Solid content of cooking water of raw rice were higher than those of parboiled rice. Hardness of uncooked PL20 & PL40 soaked for 30 min was higher than that of raw rice but that of uncookef parboiled rice soaked for 90 min was lower than that of raw rice. Springness of cooked parboile rice for initial 10 min decresed with that of cooked raw rice and then increased sharply, cooked f, r 15 min then increased slowly, cooked parboiled rice for 40 min increased more than cooked raw rice. Color differences($\Delta$I) of PT2O samples was the lowest L value of all the samples increased but a and b value decreased according to milling degree was high.

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Cytotoxicities of Hydrolyzed Crude Laminaran from Eisenia bicyclis on the SNU-1, HeLa and SW Cells (대황으로부터 추출한 crude laminaran 가수분해물의 암 세포독성)

  • Do, Jeong-Ryong;Kim, Dong-Soo;Park, Jong-Hyuk;Kim, Young-Myung
    • Korean Journal of Food Science and Technology
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    • v.38 no.6
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    • pp.793-798
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    • 2006
  • We investigated the effects on the cytotoxicity against several cancer cells of the hydrolysis and molecular weight fractionation of crude laminaran from E. bicyclis, a brown seaweed collected from Uleung island in Korea, was extracted with boiling water and then crude laminaran was prepared by ethanol precipitation of extract obtained after elimination of calcium alginate by calcium chloride. Crude laminaran was hydrolyzed by enzyme (Econase CE), acid (0.1 N HCl) and autoclaving ($121^{\circ}C$, 180 min), and the molecular weight fractions by ultrafiltration to generate molecular weight fractions. Total sugar and sulfate contents of hydrolyzed laminaran were 72.3 and 3.5% (enzyme hydrolysate), 68.5 and 3.0% (acid hydrolysate), 70.2 and 3.2% (autoclaved), and monosaccharides of which consisted of glucose (74.7-78.5%), mannose (9.9-11.5%), galactose (8.5-9.6%) and fucose (3.1-4.5%), respectively. When the cytotoxicity of hydrolyzed laminaran on SNU-1, HeLa and SW cells was evaluated by MTT assay, growth-inhibitory activity of the enzyme hydrolysate against cancer cells was higher than that of acid hydrolysate or autoclaved laminaran. Furthermore, the fraction at a molecular weight range of 10 to 50 kDa revealed higher anti-proliferative activities. The $IC_{50}$ values of 10-50 kDa fraction at a molecular weight range of 10 to 50 kDa revealed higher anti-proliferative activities. The $IC_{50}$ values of 10-50 kDa fractions on SNU-1, HeLa and SW cells were 60.4, 58.6 and 53.9 ${\mu}g/mL$ for enzymatic hydrolysate, 75.6, 73.5 and 77.4 ${\mu}g/mL$ for acid hydrolysate, and 61.7, 68.2 and 60.8 ${\mu}g/mL$ for autoclaved, respectively.

Growth and Grain Characteristics of Thin-Shelled High-Yielding Lines of Job's-tears (Coix lacryma-jobi L.) (율무 박피(薄皮) 다수성(多收性) 선발(選拔) 계통(系統)의 생육(生育) 및 종실특성(種實特性))

  • Lee, Jung-Il;Park, Jang-Hwan;Kim, Sok-Dong;Ahn, Byeong-Ok;Lee, Seung-Tack
    • Korean Journal of Medicinal Crop Science
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    • v.1 no.1
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    • pp.24-27
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    • 1993
  • This study was conducted to select thin-shelled and high-yielding lines in job's-tears. Two breeding lines of Suwon 3 and Suwon 6 were selected from the local collections. These two lines were tested and investigated on their characteristics under the field condition. The heading date of Suwon 3 and Suwon 6 was later one or two days, but the maturity date was one or two days earlier than that of check variety Kim-jejong, respectively. The number of grains per hill of Suwon 3, Suwon 6 was 50%, 49% greater and the milling rate was 3.8%, 5.6% higher than that of check variety, respectively. Althought 1000 grain weight of Suwon 3 and Suwon 6 was 20g lighter and the rate of ripeness was 6%, 12% lower, the raw grain yield was 22%, 20% higher than that of check variety, respectively. The thickness of seed coat of Suwon 3 and Suwon 6 was thiner and the hardness of seed coat was lower than that of check variety, therefore the milling time was decreased 12%, 7% compare to check variety, respectively. The crude protein contents of Suwon 3 and Suwon 6 was slightly higher and the amino acid composition of Suwon 6 was similar to Kimjejong, but Suwon 3 was lower than that of check variety.

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Effect of Thresher Drum-Speed on the Quality of the Milled Rice (탈곡기의 급동 속도가 도정 손실에 미치는 영향)

  • 정창주;고학균;이종호;강화석
    • Journal of Biosystems Engineering
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    • v.4 no.2
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    • pp.10-24
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    • 1979
  • It is understood that drum speed of threshers and the moisture content of paddy grains to be threshed, respectively, have a signific:mt effect upon rice recoveries. Threshing under an increased drum speed would give a high performance rate, which is the general practice in custom work threshing in association with the use of semiauto-t hreshers. In the connection, however, it may result in the promotion of grain cracks and brokens of the rice product after milling. No reference or determination for an opti mum drum speed of the thresher is made available for various grain moisture contents at the time of the threshing operation and for different rice varieties especially for the Tongil rice varieties. This study was Conducted to find out and determine effects of the drum speeds on grain losses. The grain loss was quantified in terms of recovery rates of rice grains after treatments. Samples of each of all treatments were taken from the grain sampling plate placed in the grain conveyor of threshers. The grain sample plate was specially provided for this experiment. The brown-rice, milling, and head-rice recJveries were tes ted in the laboratory mill, respectively. Two rice varieties, Akibare and Suweon 251, each with five levels of different moist\ulcornerure contents at harvest and six levels of different drum speeds of threshers, were selected and used for treatments in this experiment. Two conditions of materials were tested in the thresher. One condition was to thresh the experimental material immediately after cutting, referred to as the wet-material thr eshing in this study. The other was to thresh the experimental :material, dried to contain about 15-16 percent of the grain moisture under the shocking operation. This is referred to as the dry-material threshing in this study. In additioon, field measurements for the grain moistures and drum-sdeeds under actual operation practices of the traditional field threshing, were conducted with a view to comparing with results of the experimental treatments. The results of the study may be summarized as follows: 1. For threshing treatments of Japonica-type rice variety (Akibare) , the effect of drum speeds and levels of grain moisture at cutting upon brown-rice, milling, and head-rice recoveries were found statistically significant. No significant difference in these recovery rates was noticed regardless of whether the material was threshed right after cutting or after drying by the shocking operation. 2. For the Tongil-sister rice variety(Suweon 251), milling recovery for the varied drum-speed and the grain~moisture level at cutting was found statististically significant. Th milling recovery was much significant when associated with the wet-material thres\ulcornerhing compared to the dry-material threshing. 3. The optimum peripheral velocity to be maintained at the edge of teeth on the thr\ulcorneresher drum was determined and may be recommanded as that of about 12 to 13 meters per second in view of the maximum recovery rate of the milled rice. 4. The effect of the drum speed on the qualitative loss of the milled rice was much greater in the case of the Tongil variety than Japonica. This effect was also greater by the wet-material threshing than by the dry-material threshing. Therefore, to apply the wet-material threshing operation for the Tongil variety, in particular, it should be very important to introduce the kind of threshing technology which would maintain the drum speed at optimum. 5. A field survey for the actual drum speed of threshing operations for 50 threshers indicated that average peripheral velccity was 12.76m/sec., and that the range was from 10.50 to 14.90m/sec. Approximately, more than 30% of the experimented and measured threshers were being operated at speeds which exceeded the optimum speed determined and assessed in this study. Accordingly, it should be highly desirable and important to take counter-measures against these threshing practices of operational overspeed.

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Effect of Thresher Drum-Speed on the Quality of the Milled Rice (탈곡기의 급동 속도가 도정 손실에 미치는 영향)

  • Chung, Chang Joo;Koh, Hak Kyun;Lee, Chong Ho;Kang, Hwa Seug
    • Journal of Biosystems Engineering
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    • v.4 no.2
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    • pp.9-9
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    • 1979
  • It is understood that drum speed of threshers and the moisture content of paddy grains to be threshed, respectively, have a signific:mt effect upon rice recoveries. Threshing under an increased drum speed would give a high performance rate, which is the general practice in custom work threshing in association with the use of semiauto-t hreshers. In the connection, however, it may result in the promotion of grain cracks and brokens of the rice product after milling. No reference or determination for an opti mum drum speed of the thresher is made available for various grain moisture contents at the time of the threshing operation and for different rice varieties especially for the Tongil rice varieties. This study was Conducted to find out and determine effects of the drum speeds on grain losses. The grain loss was quantified in terms of recovery rates of rice grains after treatments. Samples of each of all treatments were taken from the grain sampling plate placed in the grain conveyor of threshers. The grain sample plate was specially provided for this experiment. The brown-rice, milling, and head-rice recJveries were tes ted in the laboratory mill, respectively. Two rice varieties, Akibare and Suweon 251, each with five levels of different moist?ure contents at harvest and six levels of different drum speeds of threshers, were selected and used for treatments in this experiment. Two conditions of materials were tested in the thresher. One condition was to thresh the experimental material immediately after cutting, referred to as the wet-material thr eshing in this study. The other was to thresh the experimental :material, dried to contain about 15-16 percent of the grain moisture under the shocking operation. This is referred to as the dry-material threshing in this study. In additioon, field measurements for the grain moistures and drum-sdeeds under actual operation practices of the traditional field threshing, were conducted with a view to comparing with results of the experimental treatments. The results of the study may be summarized as follows: 1. For threshing treatments of Japonica-type rice variety (Akibare) , the effect of drum speeds and levels of grain moisture at cutting upon brown-rice, milling, and head-rice recoveries were found statistically significant. No significant difference in these recovery rates was noticed regardless of whether the material was threshed right after cutting or after drying by the shocking operation. 2. For the Tongil-sister rice variety(Suweon 251), milling recovery for the varied drum-speed and the grain~moisture level at cutting was found statististically significant. Th milling recovery was much significant when associated with the wet-material thres?hing compared to the dry-material threshing. 3. The optimum peripheral velocity to be maintained at the edge of teeth on the thr?esher drum was determined and may be recommanded as that of about 12 to 13 meters per second in view of the maximum recovery rate of the milled rice. 4. The effect of the drum speed on the qualitative loss of the milled rice was much greater in the case of the Tongil variety than Japonica. This effect was also greater by the wet-material threshing than by the dry-material threshing. Therefore, to apply the wet-material threshing operation for the Tongil variety, in particular, it should be very important to introduce the kind of threshing technology which would maintain the drum speed at optimum. 5. A field survey for the actual drum speed of threshing operations for 50 threshers indicated that average peripheral velccity was 12.76m/sec., and that the range was from 10.50 to 14.90m/sec. Approximately, more than 30% of the experimented and measured threshers were being operated at speeds which exceeded the optimum speed determined and assessed in this study. Accordingly, it should be highly desirable and important to take counter-measures against these threshing practices of operational overspeed.

LCA (Life Cycle Assessment) for Evaluating Carbon Emission from Conventional Rice Cultivation System: Comparison of Top-down and Bottom-up Methodology (관행농 쌀 생산체계의 탄소배출량 평가를 위한 전과정평가: top-down 방식의 국가평균값과 bottom-up 방식의 사례분석값 비교)

  • Ryu, Jong-Hee;Jung, Soon Chul;Kim, Gun-Yeob;Lee, Jong-Sik;Kim, Kye-Hoon
    • Korean Journal of Soil Science and Fertilizer
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    • v.45 no.6
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    • pp.1143-1152
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    • 2012
  • We established a top-down methodology to estimate carbon footprint as national mean value (reference) with the statistical data on agri-livestock incomes in 2007. We also established LCI (life cycle inventory) DB by a bottom-up methodology with the data obtained from interview with farmers from 4 large-scale farms at Gunsan, Jeollabuk-do province to estimate carbon footprint in 2011. This study was carried out to compare top-down methodology and bottom-up methodology in performing LCA (life cycle assessment) to analyze the difference in GHGs (greenhouse gases) emission and carbon footprint under conventional rice cultivation system. Results of LCI analysis showed that most of $CO_2$ was emitted during fertilizer production and rice cultivation, whereas $CH_4$ and $N_2O$ were mostly emitted during rice cultivation. The carbon footprints on conventional rice production system were 2.39E+00 kg $CO_2$-eq. $kg^{-1}$ by top-down methodology, whereas 1.04E+00 kg $CO_2$-eq. $kg^{-1}$ by bottom-up methodology. The amount of agro-materials input during the entire rice cultivation for the two methodologies was similar. The amount of agro-materials input for the bottom-up methodology was sometimes greater than that for top-down methodology. While carbon footprint by the bottom-up methodology was smaller than that by the top-down methodology due to higher yield per cropping season by the bottom-up methodology. Under the conventional rice production system, fertilizer production showed the highest contribution to the environmental impacts on most categories except GWP (global warming potential) category. Rice cultivation was the highest contribution to the environmental impacts on GWP category under the conventional rice production system. The main factors of carbon footprints under the conventional rice production system were $CH_4$ emission from rice paddy field, the amount of fertilizer input and rice yield. Results of this study will be used for establishing baseline data for estimating carbon footprint from 'low carbon certification pilot project' as well as for developing farming methods of reducing $CO_2$ emission from rice paddy fields.

Monitoring of Pathogens in Cultured Fish of Korea for the Summer Period from 2000 to 2006 (2000년~2006년 하절기 양식어류의 병원체 감염현황)

  • Jung, Sung-Hee;Kim, Jin-Woo;Do, Jeong-Wan;Choi, Dong-Lim;Jee, Bo-Young;Seo, Jung-Seo;Park, Myoung-Ae;Cho, Mi-Young;Kim, Myoung-Sug;Choi, Hye-Sung;Kim, Yi-Cheong;Lee, Joo-Seok;Lee, Chang-Hoon;Bang, Jong-Deuk;Park, Mi-Seon
    • Journal of fish pathology
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    • v.19 no.3
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    • pp.207-214
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    • 2006
  • Diagnostic monitoring in fish farms with land-based tanks and net cases was conducted in eastern, western, southern and Jeju island of Korea for the summer period from 2000 to 2006. Total 3,518-fish samples of marine and freshwater fishes in 25 fish species were tested for pathogens. Fish species tested were olive flounder (Paralichthys olivaceus), fleshy prawn (Fenneropenaeus chinensis Osbeck), black rockfish (Sebastes schlegeli), rock bream (Oplegnathus fasciatus), red sea bream (Pagrus major), black seabream (Acanthopagrus schlegeli), sea bass (Lateolabrax japinicus), gray mullet (Mugil cephalus), rainbow trout (Onchorhynchus mykiss) and others. The infection rates by bacterial pathogens in the years of 2000, 2001, 2002, 2003, 2004, 2005 and 2006 were 22.4%, 34.5%, 14.1%, 15.3%, 17.7%, 13.5% and 5%, respectively. The infection rates by parasitic pathogens were 20%, 33.8%, 12.4%, 14.1%, 9.2%, 10.5% and 10.7%, respectively. The infection rates by viral pathogens were 22.4%, 13.5%, 10.3%, 5.4%, 9.7%, 10.2% and 15.8%, respectively. The infection rates by mixed pathogens were 10.3%, 0%, 44.9%, 50.9%, 31.9%, 38.4% and 39.6%, respectively. The rates of mixed infections were very low until 2001. The rates were higher than those of singer infections from 2002 to 2006. During the diagnostic monitoring from 2000 to 2006, the main bacterial pathogens were Vibrio (41.2%) and Streptococcus (28.8%). The infection rate by protozoa (85.7%) mainly including Scuticociliates and Trichodina was highest. The infection rate by viral necrosis virus (VNNV, 42.2%) was the highest of the viral pathogens.