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Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

Accuracy of 5-axis precision milling for guided surgical template (가이드 수술용 템플릿을 위한 5축 정밀가공공정의 정확성에 관한 연구)

  • Park, Ji-Man;Yi, Tae-Kyoung;Jung, Je-Kyo;Kim, Yong;Park, Eun-Jin;Han, Chong-Hyun;Koak, Jai-Young;Kim, Seong-Kyun;Heo, Seong-Joo
    • The Journal of Korean Academy of Prosthodontics
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    • v.48 no.4
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    • pp.294-300
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    • 2010
  • Purpose: The template-guided implant surgery offers several advantages over the traditional approach. The purpose of this study was to evaluate the accuracy of coordinate synchronization procedure with 5-axis milling machine for surgical template fabrication by means of reverse engineering through universal CAD software. Materials and methods: The study was performed on ten edentulous models with imbedded gutta percha stoppings which were hidden under silicon gingival form. The platform for synchordination was formed on the bottom side of models and these casts were imaged in Cone beam CT. Vectors of stoppings were extracted and transferred to those of planned implant on virtual planning software. Depth of milling process was set to the level of one half of stoppings and the coordinate of the data was synchronized to the model image. Synchronization of milling coordinate was done by the conversion process for the platform for the synchordination located on the bottom of the model. The models were fixed on the synchordination plate of 5-axis milling machine and drilling was done as the planned vector and depth based on the synchronized data with twist drill of the same diameter as GP stopping. For the 3D rendering and image merging, the impression tray was set on the conbeam CT and pre- and post- CT acquiring was done with the model fixed on the impression body. The accuracy analysis was done with Solidworks (Dassault systems, Concord, USA) by measuring vector of stopping’s top and bottom centers of experimental model through merging and reverse engineering the planned and post-drilling CT image. Correlations among the parameters were tested by means of Pearson correlation coefficient and calculated with SPSS (release 14.0, SPSS Inc. Chicago, USA) ($\alpha$ = 0.05). Results: Due to the declination, GP remnant on upper half of stoppings was observed for every drilled bores. The deviation between planned image and drilled bore that was reverse engineered was 0.31 (0.15 - 0.42) mm at the entrance, 0.36 (0.24 - 0.51) mm at the apex, and angular deviation was 1.62 (0.54 - 2.27)$^{\circ}$. There was positive correlation between the deviation at the entrance and that at the apex (Pearson Correlation Coefficient = 0.904, P = .013). Conclusion: The coordinate synchronization 5-axis milling procedure has adequate accuracy for the production of the guided surgical template.

Distribution of Zooplankton by ADCP's Echo Intensity in the Coastal Water used Yellow Loess (다층 도플러 유속계(ADCP)를 이용한 황토 살포 해역의 플랑크톤 평가)

  • Park, Ju-Sam;Choo, Hyo-Sang;Moon, Sung-Ryong
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.16 no.2
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    • pp.141-151
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    • 2010
  • Harmful algal blooms (HABs), commonly known as red tides, are aquatic phenomena caused by the rapid growth and accumulation of certain microalgae, which can lead to marked discoloration of surface waters, and severe impacts on public health, commerce, and the environment. In South Korea, the red tides have been a serious and recurrent problem, especially along the south coast. Plenty of yellow loess was used to control an outbreak of the red tides for 15 years from 1996 until now. Yellow loess was almost sprayed in the vicinity of a large fish farming industry. In this research, the distribution characteristics and density distribution of zooplankton were investigated in autumn (Oct. 2008) and spring (Apr. 2009) using volume backscattering strength (SV) calculated by the zooplankton collected with north pacific standard (NORPAC) net and the echo intensity measured with ADCP at stations on the study area in the spraying ocean of yellow loess (SOYL), and the non-spraying ocean of yellow ocean (NOYL) by the red tide generating every year. The species number and the individuals per unit volume of the zooplankton collected in NOYL was high and it which was collected in SOYL was low. As a result of comparing the volume backscattering strength ($SV_c$) calculated by species and length of the zooplankton collected with NORPAC net with the volume backscattering strength ($SV_m$) calculated by the echo intensity measured with ADCP at stations on the study area, although $SV_c$ and $SV_m$ of NOYL were generally in agreement, $SV_m$ of SOYL was higher than $SV_c$ 4.3dB, i.e. ADCP is greatly influenced by suspended solid in SOYL. The horizontal distribution map of $SV_m$ at the study area in autumn (Oct. 2008) and spring (Apr. 2009) was drawn. $SV_m$ of SOYL is higher than NOYL and autumn is higher than spring. $SV_m$ can suppress the overestimate or underestimate of $SV_c$.

Effects of Total Mixed Fermentation Feeds Based on Rice-straw and Six Forage Crops on the Productivity of Holstein Cows (청예사료작물과 볏짚 위주의 완전배합발효사료 급여가 Holstein 착유우의 생산성에 미치는 영향)

  • Lee, H. J.;Kim, H. S.;Ki, K. S.;Jeong, H. Y.;Baek, K. S.;Kim, J. S.;Cho, K. K.;Cho, J. S.;Lee, H. G.;Woo, J. H.;Choi, Y. J.
    • Journal of Animal Science and Technology
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    • v.45 no.1
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    • pp.69-78
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    • 2003
  • This experiment was carried out to evaluate the value of total mixed fermentation feeds(TMFF) as completely mixed ration and to observe the effect of various kinds of TMFF on the palatability, feed intake, and milk performance in Holstein cows. The dry matter (DM) content of TMFF used in the experiment was 23.98-28.42% range, and CP, TDN, ADF and NDF were 16.2${\sim}$19.2%, 58.3-65.1%, 34.4-39.6% and 46.9${\sim}$49.9% levels, respectively. The relative feed value (RFV) in rape-, alfalfa-, grass-, oat-, corn-TMFF groups were 138.6, 133.9, 116.5, 111.8, 111.4 and 108.1, respectively. Among these groups, RFV of rye-TMFF group was lowest. Dry matter disappearance(DMD) showed 0.8${\sim}$.9% to the all kinds of TMFF groups. The pH was 3.89${\sim}$.87 and $NH_3$-N concentration was 6.93-8.66 mg/$d\ell$. The acetic acid concentration in the raw material of TMFF showed low level of 0.19${\sim}$0.57%, lactic acid showed high level of 1.17${\sim}$3.21% and butyric acid was very high as 0.03${\sim}$0.32%. Therefore, these results provide evidence that the quality of TMFF was not so bad. In the daily fresh matter intake on the alfalfa-, grass-, rape-, corn-, oats- and rye-TMFF were showed 62.85, 60.48, 58.04, 57.11, 54.61 and 45.74 kg respectively. All TMFF showed high palatability as daily dry matter intake of 1.95 to 2.90% by body weight of experimental cows. Body condition score(BCS) was gradually increased in during 60 days of the experiment term. Average daily gain(ADG) showed about 140.0${\sim}$326.7g. In alfalfa-TMFF group, the ADG was higher than in the other groups (p<0.05). Also, the increase in BCS was observed in grass-TMFF group (3.07 to 3.34) and rye-TMFF group was decreased in 3.07 to 3.34 (p<0.05). The milk yield appropriately showed a range of 16.16${\sim}$18.95 kg in all groups. Among these groups, alfalfa-TMFF group was highest(P<0.05). Average milk fat contents showed high levels of 4.06${\sim}$4.79% and the level was high in order of rape-, grass-, corn-, alfalfa-, rye- and oats-TMFF. Milk protein was highest in forage-TMFF and level of lactose in milk was approximately 4.56% in overall groups. Solid non fat(SNF) and total solid(TS) contents were 8.75% and 12.8%, respectively. However, milk composition was not significantly affected by TMFF.

Measurement of the Levels of IgG Subclasses Reactive to Salmonella typhi in the Sera of Patients with Typhoid Fever (장티푸스환자의 혈청내 Salmonella typhi에 대한 IgG subclass항체의 분포)

  • Kim, Young-Jung;Hwang, Eung-Soo;Kang, Jae-Seung;Cha, Chang-Yong;Chang, Woo-Hyun;Kim, Yoon-Won;Cho, Min-Ki;Min, Chang-Hong
    • The Journal of the Korean Society for Microbiology
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    • v.21 no.4
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    • pp.447-453
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    • 1986
  • To diagnose the typhoid fever rapidly and accurately in clinically suspected patients, the levels of IgG subclass antibody were measured by enzyme-linked immunosorbent assay(ELISA). With symptom, blood culture and agglutination test, tested persons were categorized into 6 groups as typhoid fever, FUO, paratyphi A or B, other bacterial infctions, cancers, and control. ELISA was performed on the polyvinyl chloride plates coated with killed whole cell($10^8\;cell/ml$) of S. typhi 0901W by poly-L-lysine applied as binding substance (and polyvinyl chloride as solid phase). The distribution of the level of IgG subclass antibodies in each group was analyzed and compared with other groups. The results obtained were summarized as follow: 1. The optimal dilution of the sera from patients with typhoid fever was 1:160, and those of the sheep anti-human IgG subclass and the peroxidase conjugated rabbit anti-sheep IgG were 1:4000 and 1:5000, respectively. 2. The absorbance levels of IgG subclass in the sera of typhoid fever patients were as follows; a) IgG1 value is $0.439{\pm}0.110$ b) IgG2 value is $0.416{\pm}0.165$ c) IgG3 value is $0.449{\pm}0.145$ d) IgG4 value is $0.525{\pm}0.154$ IgG subclass levels in the sera of typhoid patients were much higher than in control group and patient with paratyphi A or B as well as other infectious diseases. The sensitivity and the specificity in differential diagnosis of typhoid fever and other febrile diseases were 92% and 79% in the assay of IgG1 respectively, whereas those in the assay of IgG2 were 97% and 72%, respectively (above absorbance 0.3). 3. The absorbance levels of IgG subclass in the serial sera of typhiod fever patients tend to decrease to the level of absorbance 0.3 in 10 months from the onset of illness. 4. The order of absorbance levels of IgG subclass in the serum of each group were typhoid fever, paratyphi A or B, other infectious diseases, control and cancer. 5. For the serodiagnosis of typhoid fever against other febrile diseases, the sensitivity and the specificity in the assay of IgG2 activity were 76% and 93% in absorbance 0.4, respectively. 6. In the distribution of the level of each IgG subclass in the sera of FUO patients which were suspected of typhoid fever, the positive rate was ranged from 36% to 82%. This suggest that more than 50% of FUO patients are caused by S. typhi.

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Expression of Oncogene Product in the Colorectal Carcinoma (결장암 및 직장암에서 암유전자 산물의 발현)

  • Shim, Young-Ran;Jang, Woo-Young;Choi, Kyoung-Chan;Choi, Joon-Hyuk;Choi, Won-Hee;Shim, Min-Chul
    • Journal of Yeungnam Medical Science
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    • v.12 no.2
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    • pp.210-225
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    • 1995
  • The expression of $p62^{c-myc}$ and $p21^{ras}$ can be seen in many solid tumor, but the pattern and incidence of expression were different according to organ, countries, and examiners, thus it is not definitely defined. Total 67 colorectal carcinoma in paraffin sections are analysed by immunohistochemically for evaluation of the $p62^{c-myc}$ and $p21^{ras}$ expression according to the age, sex, chief complaints, location, differentiation, modified Dukes stage, using the specific monoclonal antibodies. The results were summarized as follows : The age of patients ranged from 32 years to 82 years. The mean age was 57.6 years. The expression of $p62^{c-myc}$ and $p21^{ras}$ was not correlated with age. Male was 29 cases(43.3%) and female was 38 cases(56.7%). The male to female ratio was 1:1.31. The expression of $p21^{ras}$ was increased in female(p<0.05). Abdominal pain(43.7%) was the most frequent chief complaint. The most frequent tumor location was rectum(44.8%). The expression of $p62^{c-myc}$ was increased in the rectum(p<0.05). The 65 cases(97.0%) out of 67 cases showed positive reaction of $p62^{c-myc}$ in the nucleus, cytoplasmic membrane, and cytoplasm. The 62 cases(92.5%) out of 67 cases showed positive reaction of $p21^{ras}$ in the cytoplasmic membrane and cytoplasm. The positive rate of $p62^{c-myc}$ and $p21^{ras}$ was 97.0% and 91.4% in well differentiated adenocarcinoma, 100.0% and 95.0% in moderately differentiated adenocarcinoma, 90.0% and 90.0% in poorly differentiated adenocarcinoma, 100.0% and 100.0% in mucinous carcinoma. The positive rate of $p62^{c-myc}$ and $p21^{ras}$ was 94.1% and 88.2% in Dukes stage $B_1$, 96.0% and 96.0% in Dukes stage $B_2$, 100.0% and 100.0% in Dukes stage $C_1$, 100.0% and 88.9% in Dukes stage $C_2$, and 100.0% and 100.0% in Dukes stage D. The expression of $p62^{c-myc}$ in metastatic colorectal carcinoma showed diffuse and strongly positive reaction than primary colorectal carcinoma. The expression of $p21^{ras}$ in primary colorectal carcinoma showed diffuse and strongly positive reaction than metastatic colorectal carcinoma.

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Preliminary Report of the $1998{\sim}1999$ Patterns of Care Study of Radiation Therapy for Esophageal Cancer in Korea (식도암 방사선 치료에 대한 Patterns of Care Study ($1998{\sim}1999$)의 예비적 결과 분석)

  • Hur, Won-Joo;Choi, Young-Min;Lee, Hyung-Sik;Kim, Jeung-Kee;Kim, Il-Han;Lee, Ho-Jun;Lee, Kyu-Chan;Kim, Jung-Soo;Chun, Mi-Son;Kim, Jin-Hee;Ahn, Yong-Chan;Kim, Sang-Gi;Kim, Bo-Kyung
    • Radiation Oncology Journal
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    • v.25 no.2
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    • pp.79-92
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    • 2007
  • [ $\underline{Purpose}$ ]: For the first time, a nationwide survey in the Republic of Korea was conducted to determine the basic parameters for the treatment of esophageal cancer and to offer a solid cooperative system for the Korean Pattern of Care Study database. $\underline{Materials\;and\;Methods}$: During $1998{\sim}1999$, biopsy-confirmed 246 esophageal cancer patients that received radiotherapy were enrolled from 23 different institutions in South Korea. Random sampling was based on power allocation method. Patient parameters and specific information regarding tumor characteristics and treatment methods were collected and registered through the web based PCS system. The data was analyzed by the use of the Chi-squared test. $\underline{Results}$: The median age of the collected patients was 62 years. The male to female ratio was about 91 to 9 with an absolute male predominance. The performance status ranged from ECOG 0 to 1 in 82.5% of the patients. Diagnostic procedures included an esophagogram (228 patients, 92.7%), endoscopy (226 patients, 91.9%), and a chest CT scan (238 patients, 96.7%). Squamous cell carcinoma was diagnosed in 96.3% of the patients; mid-thoracic esophageal cancer was most prevalent (110 patients, 44.7%) and 135 patients presented with clinical stage III disease. Fifty seven patients received radiotherapy alone and 37 patients received surgery with adjuvant postoperative radiotherapy. Half of the patients (123 patients) received chemotherapy together with RT and 70 patients (56.9%) received it as concurrent chemoradiotherapy. The most frequently used chemotherapeutic agent was a combination of cisplatin and 5-FU. Most patients received radiotherapy either with 6 MV (116 patients, 47.2%) or with 10 MV photons (87 patients, 35.4%). Radiotherapy was delivered through a conventional AP-PA field for 206 patients (83.7%) without using a CT plan and the median delivered dose was 3,600 cGy. The median total dose of postoperative radiotherapy was 5,040 cGy while for the non-operative patients the median total dose was 5,970 cGy. Thirty-four patients received intraluminal brachytherapy with high dose rate Iridium-192. Brachytherapy was delivered with a median dose of 300 cGy in each fraction and was typically delivered $3{\sim}4\;times$. The most frequently encountered complication during the radiotherapy treatment was esophagitis in 155 patients (63.0%). $\underline{Conclusion}$: For the evaluation and treatment of esophageal cancer patients at radiation facilities in Korea, this study will provide guidelines and benchmark data for the solid cooperative systems of the Korean PCS. Although some differences were noted between institutions, there was no major difference in the treatment modalities and RT techniques.

Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

Skeletal relapse and dental change during intermaxillary fixation after mandibular setback (외과적 하악 후퇴술 후 악간고정기간 중의 골격성 재발과 치열의 변화)

  • Chang, Chong-On
    • The korean journal of orthodontics
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    • v.29 no.4 s.75
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    • pp.457-466
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    • 1999
  • It has been reported that skeletal relapse and dental change after mandibular setback do occur not only after intermaxillary fixation(IMF) removal but also during IMF The side effects of skeletal relapse during IMF have clinical importance because they can cause many Postoperative orthodontic Problems. Generally, the Prevention of solid union between segments, compensatory tooth movement, anterior openbite, etc. have been cited as the side effects of jaw displacement. The purpose of this study was to evaluate the skeletal relapse and dental change during IMF. The material consisted of 28 patients who were treated by BSSRO(bilateral sagittal split ramus osteotomy), wire osteosynthesis, IMF for correction of mandibular prognathism. Through cephalometric analysis, the amount and direction of surgical movement, skeletal relapse and dental change during IMF were measured. The correlation between surgical movement and skeletal relapse, between skeletal relapse and dental changes were evaluated. The following conclusions were obtained; 1. Distal segment was repositioned backward and upward, proximal segment showed clockwise rotation during surgery. 2. During ]m, anterior portion of distal segment was displaced backward and posterior portion was displaced upward. Proximal segment was displaced upward with forward movement of p-Go(gonion of proximal segment). Backward surgical movement of p-GO was significantly correlated with forward displacement of p-Go. 3. Overjet and overbite were not changed during IMF. The compensatory tooth movements during IMF were characterized by retroclination of upper incisors md retroclination, extrusion of lower incisors. These compensatory tooth movements had statistically significant correlation with upward displacement of d-Go (gonion of distal segment).

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A Survey on the Status and Strategy of Swine Manure Utilization in the Gyeongnam (경남지역의 양돈분뇨 자원화 이용과 개선방안에 관한 실태조사)

  • Kim, D.H.;Shin, J.K.;Han, J.C.
    • Journal of Animal Environmental Science
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    • v.16 no.1
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    • pp.1-12
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    • 2010
  • This survey was conducted to investigate the status and strategy of swine manure utilization of 109 swine farms in the Gyeongnam, Korea. The personal properties of owner, types of swine buildings, facilities and equipment for manure management, conditions for manure recycling and farming for recycling resources were surveyed. Age of farm owners were occupied as 44.1% for 50s followed by the 60s with one-forth and 40s with 22.9%. Educational background of farm owners, a high school graduate makes up the largest proportion of farm owners followed by a college graduation with 35.8%. The swine manure collection methods were occupied as 34.9% with totally slurry system and more than 50% slurry system with 34.9% of farms. The manure management cost per ton were occupied as more than two-third with 10,000 won~15,000 won. The cost will pay for manure management, 10,000 won~15,000 won per ton makes up the largest proportion of farm owners. Separator, loader and vehicle to collection, transportation of liquid manure were occupied as 72.5%, 44% and 10.1%, respectively. Recognition of the farming for recycling resources were occupied as 37.6%, however, 25.8% of swine farm owners don't know that. More than sixty percent of swine farms will take a recycling system according to the farming for recycling resources. Conclusively, we have a suggestion in order to promotion of the farming for recycling resources in the Gyeongnam with increasing the portion of recycling of swine manure in each county and revitalizing the marketing of the liquid and solid swine manure fertilizers.