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Development of Analytical Method for Detection of Fungicide Validamycin A Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Validamycin A의 시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.22-29
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    • 2019
  • Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

Studies on the ecological variations of rice plant under the different seasonal cultures -I. Variations of the various agronomic characteristics of rice plant under the different seasonal cultures- (재배시기 이동에 의한 수도의 생태변이에 관한 연구 -I. 재배시기 이동에 의한 수도의 실용제형질의 변이-)

  • Hyun-Ok Choi
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.3
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    • pp.1-40
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    • 1965
  • To measure variations in some of the important agronomic characteristics of rice varieties under shifting of seedling dates, this study has been carried out at the Paddy Crop Division of Crop Experiment Station(then Agricultural Experiment Station) in Suwon for the period of three years 1958 to 1960. The varieties used in this study were Kwansan, Suwon #82, Mojo, Paltal and Chokwang, which have the different agronomic characteristics such as earliness and plant type. Seeds of each variety were sown at 14 different dates in 10-day interval starting on March 2. The seedlings were grown on seed bed for 30, 40, 50, 60, 70 and 80 days, respectively. The results of this study are as follows: A. Heading dates. 1. As the seeding date was delayed, the heading dates was almost proportionally delayed. The degree of delay was higher in early varieties and lower in late varieties and the longer the seedling stage, the more delayed the heading date. 2. Number of days to heading was proportionally lessened as seeding was delayed in all the varieties but the magnitude varied depending upon variety. In other words, the required period for heading in case of late planting was much shortened in late variety compared with early one. Within a variety, the number of days to heading was less shortened as the seedling stage was prolonged. Early variety reached earlier than late variety to the marginal date for the maximum shortening of days to heading and the longer the seeding stage, the limitted date came earlier. There was a certain limit in seeding date for shortening of days to heading as seeding was delayed, and days to heading were rather prolonged due to cold weather when seeded later than that date. 3. In linear regression equation, Y=a+bx obtained from the seeding dates and the number of days to heading, the coefficient b(shortening rate of days to heading) was closely correlated with the average number of days to heading. That is, the period from seeding to heading was more shortened in late variety than early one as seeding was delayed. 4. To the extent that the seedling stage is not so long and there is a linear relationship between delay of seeding and shortening of days to heading, it might be possible to predict heading date of a rice variety to be sown any date by using the linear regression obtained from variation of heading dates under the various seeding dates of the same variety. 5. It was found out that there was a close correlation between the numbers of days to heading in ordinary culture and the other ones. When a rice variety was planted during the period from the late part of March to the middle of June and the seedling ages were within 30 to 50 days, it could be possible to estimate heading date of the variety under late or early culture with the related data of ordinary culture. B. Maturing date. 6. Within (he marginal date for maturation of rice variety, maturing date was proportionally delayed as heading was delayed. Of course, the degree of delay depended upon varieties and seedling ages. The average air temperature (Y) during the ripening period of rice variety was getting lower as the heading date. (X) was delayed. Though there was a difference among varieties, in general, a linear regression equation(y=25.53-0.182X) could be obtained as far as heading date were within August 1 to September 13. 7. Depending upon earliness of a rice variety, the average air temperature during the ripening period were greatly different. Early variety underwent under 28$^{\circ}C$ in maximum while late variety matured under as low as 22$^{\circ}C$. 8. There was a highly significant correlation between the average air temperature (X) during the ripening period, and number of day (Y) for the maturation. And the relationship could be expressed as y=82.30-1.55X. When the average air temperature during the period was within the range of 18$^{\circ}C$ to 28$^{\circ}C$, the ripening period was shortened by 1.55 days with increase of 1$^{\circ}C$. Considering varieties, Kwansan was the highest in shortening the maturing period by 2.24 days and Suwon #82 was the lowest showing 0.78 days. It is certain that ripening of rice variety is accelerated at Suwon as the average air temperature increases within the range of 18$^{\circ}C$ to 28$^{\circ}C$. 9. Between number of days to heading (X) related to seeding dates and the accumulated average air temperature (Y) during the ripening period, a positive correlation was obtained. However, there was a little difference in the accumulated average air temperature during the ripening period even seeding dates were shifted to a certain extent. C. Culm- and ear-lengths. 10. In general all the varieties didn't show much variation in their culm-lengths in case of relatively early seeding but they trended to decrease the lengths as seeding was delayed. The magnitude of decreasing varied from young seedlings to old ones. Young seedlings which were seeded during May 21 to June 10 didn't decrease their culm-lengths, while seedlings old as 80 days decreased the length though under ordinary culture. 11. Variation in ear-length of rice varieties show the same trend as the culm-length subjected to the different seeding dates. When rice seedlings aged from 30 to 40 days, the ear-length remained constant but rice plants older than 40 days obviously decreased their ear-lengths. D. Number of panicles per hill. 12. The number of panicles per hill decreased up to a certain dates as seeding was delayed and then again increased the panicles due to the development of numerous tillers at the upper internodes. The seeding date to reach to the least number of panicles of rice variety depended upon the seedling ages. Thirty- to 40-day seedlings which were seeded during May 31 to June 10 developed the lowest number of panicles and 70- to 80-day seedlings sown for the period from April 11 to April 21 reached already to the minimum number of panicles. E. Number of rachillae. 13. To a certain seeding date, the number of rachillae didn't show any variation due to delay of seeding but it decreased remarkably when seeded later than the marginal date. 14. Variation in number of rachillae depended upon seedling ages. For example, 30- to 40-day old seedlings which, were originally seeded after May 31 started to decrease the rachillae. On the other hand, 80-day old seedlings which, were seeded on May 1 showed a tendency to decrease rachillae and the rice plant sown on May 31 could develop narrowly 3 or 4 panicles. F. Defective grain and 1.000-grain weights. 15. Under delay of the seeding dates, weight of the defective grains gradually increased till a certain date and then suddenly increased. These relationships could be expressed with two different linear regressions. 16. If it was assumed that the marginal date for ripening was the cross point of these two lines, the date seemed. closely related with seedling ages. The date was June 10- in 30- to 40-day old seedlings but that of 70- to 80-day old seedlings was May 1. Accordingly, the marginal date for ripening was getting earlier as the seedling stage was prolonged. 17. The 1.000-grain weight in ordinary culture was the heaviest and it decreased in both early and late cultures. G. Straw and rough rice weights. 18. Regardless of earliness of variety, rice plants under early culture which were seeded before March 22 or April 1 did not show much variation in straw weight due to seedling ages but in ordinary culture it gradually decreased and the degree was became greater in late culture. 19. Relationship between seeding dates (X) and grain weight related to varieties and seedling ages, could be expressed as a parabola analogous to a line (Y=77.28-7.44X$_1$-1.00lX$_2$). That is, grain yield didn't vary in early culture but it started to decrease when seeded later than a certain date, as seeding was delayed. The variation was much greater in cases of late planting and prolongation of seedling age. 20. Generally speaking, the relationship between grain yield (Y) and number of days to heading (X) was described with linear regression. However, the early varieties were the highest yielders within the range of 60 to 110, days to heading but the late variety greatly decreased its yield since it grows normally only under late culture. The grain yield, on the whole, didn't increase as number of days to heading exceeded more than 140 days.

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Factors Affecting the Formation of Iodo-Trihalomethanes during Chlorination in Drinking Water Treatment (정수처리에서 염소 처리시 요오드계 트리할로메탄류 생성에 영향을 미치는 인자들)

  • Son, Hee-Jong;Yoom, Hoon-Sik;Kim, Kyung-A;Song, Mi-Jeong;Choi, Jin-Taek
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.8
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    • pp.542-548
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    • 2014
  • Effects of bromide ($Br^-$) and iodide ($I^-$) concentrations, chlorine ($Cl_2$) doses, pH, temperature, ammonia nitrogen concentrations, reaction times and water characteristics on formation of iodinated trihalomethanes (I-THMs) during oxidation of iodide containing water with chlorine were investigated in this study. Results showed that the yields of I-THMs increased with the high bromide and iodide level during chlorination. The elevated pH significantly increased the yields of I-THMs during chlorination. The formation of I-THMs was higher at $20^{\circ}C$ than $4^{\circ}C$, $10^{\circ}C$ and $30^{\circ}C$. In chloramination study, addition of ammonium chloride ($NH_4Cl$) markedly increased the formation of I-THMs. Among the water samples collected from seven water sources including wastewater treatment plant (WWTP) effluent water (EfOM water), prepared humic containing water (HA water) and algal organic matter (AOM) containing water (AOM water), EfOM water generated the highest yields of I-THMs ($12.31{\mu}g/mg$ DOC), followed by HA water ($4.96{\mu}g/mg$ DOC), while AOM water produced the lowest yields of I-THMs ($0.99{\mu}g/mg$ DOC). $SUVA_{254}$ values of EfOM water, HA water and AOM water were $1.38L/mg{\cdot}m$, $4.96L/mg{\cdot}m$ and $0.97L/mg{\cdot}m$, respectively. The I-THMs yields had a low correlation with $SUVA_{254}$ values ($r^2$ = 0.002).

Effects of Dietary Activated Charcoal Mixed with Wood Vinegar on Quality and Chemical Composition of Egg in Laying Hens (목초액 함유 활성탄의 급여가 산란계에서 계란의 품질과 화학적 조성에 미치는 영향)

  • 김관응;유선종;안병기;조태수;안병준;최돈하;강창원
    • Journal of Animal Science and Technology
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    • v.48 no.1
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    • pp.59-68
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    • 2006
  • This experiment was conducted to investigate the effects of dietary supplementation of activated charcoal (AC) mixed with wood vinegar on performance and egg quality in laying hens. A total of one hundred ninety two, 56-wk-old Lohmann brown laying hens were divided into four groups, consisting four replicates of 12 birds each and fed one of the four experimental diets containing AC 0%, AC 0.5%, AC 1%, AC 2% for 5 wks. The blood profiles and contents of total lipid and cholesterol, fatty acid profiles in egg yolk were determined. There were no significant differences in laying performance, feed intake and vitelline membrane strength among the treatments. The eggshell breaking strength and Haugh unit were significantly increased in 2% AC group compared to the other groups (P<0.05). Egg yolk index in 2% AC group was significantly higher (P<0.05) than those of the control and 0.5% AC group and yolk color was significantly improved by the dietary AC (P<0.05). The levels of serum total cholesterol, HDL-cholesterol and enzyme activities were not influenced by feeding AC. Total lipid of egg yolk in 1 % and 2% AC groups was significantly decreased (P<0.05) compared to that of the control, although there was no significant difference in yolk cholesterol. In conclusion, the addition of activated charcoal with wood vinegar in layer diet resulted in improving egg quality by means of enhancing eggshell breaking strength, Haugh unit, yolk index and yolk color.

Pretreatment prognostic Factors in Early Stage Caricinoma of the Uterine Cervix (초기 자궁 경부암에서 치료전 예후 인자)

  • Kim, Mi-Sook;Hua, Sung-Whan
    • Radiation Oncology Journal
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    • v.10 no.1
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    • pp.59-67
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    • 1992
  • From March 1979 through December 1986, 124 patients with early stage carcinoma of the uterine cervix received curative radiation therapy. According to FIGO classification, 35 patients were stage IB and 89 were stge II A. In stage IB, five year locoregional control, five year disease free survival, and five year overall survival was $79.0\%$, $76.4\%$ and $81.8\%$, respectively. In stage II A, five year locoregional control, five year disease free survival, and five year overall survival were $78.0\%$, $66.8\%$, and $72.1\%$, respectively. To identify prognostic factors, pretreatment parameters including age, ECOG performance status, number of pregnancies, history of diabetes mellitus and hypertension, histology, size and shape of primary tumor, CT findings and blood parameters were retrospectively analyzed in terms of locoregional control, disease free survival and overall survival using univariate analysis and multivariate analysis. In univariate analysis, tumor size on physicai examination and rectal invasion on CT significantly affected locoregional control, disease free survival and overall survival. Parametrial involvement on CT was a significant prognostic factor on locoregional control and disease free survival. Hemoglobin level affected disease free survival and overall survival. Histology and age were significant prognostic factors on locoregional control. In multivariate analysis excluding CT finding, tumor size on physical examination was a significant factor in terms of locoregioal control and overall survival. Hemoglobin level was significant in terms of disease free survival. In multivariate analysis including CT, histology was a prognostic factor on locoregional control and disease free survival. Hemoglobin level and rectal invasion on CT were significant factors on locoregional control.

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An Observation Study on the Health Benefits of Fermented Milk in Relation to Gastrointestinal Diseases Prevention in Korean (유산균발효유(乳酸菌醱酵乳)의 음용(飮用)이 소화기질환(消化器疾患) 예방(豫防)에 미친 효과(效果)에 관한 조사연구(調査硏究))

  • Lee, Won-Chang;Yoon, Yoh-Chang
    • Journal of Dairy Science and Biotechnology
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    • v.14 no.1
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    • pp.57-69
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    • 1996
  • This study was desiged to carry out an observation study on the cognitive level of health benefitis of fermented milk and subsequntly, on prevention of gastrointestinal diseases for the consumers in Korea. Data used in this study were collected from two different source ; 1) 987 university students living in Seoul, were selected randomly and interviwed induvidual from May 25 to September 30 1994, to investigate the awareness status as a consomer of fermented milk, and 2) health benefits of fermented milk with respect to prevention gastric intestinal diseases such as typhoid fever, paratyphoid fever and bacillary dysentery in Korea with the raw data from the Yearbook of Health and Social Statistics by Ministry of Health and Social Affairs (1976${\sim}$1995) and Ministry of Agriculture, Forestry & Fisheries (1976${\sim}$1995), Republic of Korea. The results of this study were as follows : The effects of femented milk on health appeared to be attributed to taking care of an environment of the gastrointestinal tract regarding diarrhea, constipation and digestion, with showing 75.1% of male and 71.1% of female of university students in Seoul answered positively, The correlation coefficients of statistics between amounts of consumption per capita of fermented milk and incidence rates of gastrointestinal diseases during the period from 1975 to 1994 in the whole country was r = -0.308 (p<0.05). those of Seoul a major comsuming area of fermented milk in the country and Kangwon province, a minor consuming area were r = -0.704 (p<0.01) and r = +0.262 (n.s.), respectively. In conclusion, the results obtained in this study suggest that fermented milk exert its effect on gastrointestinal tract. Furthermore, the results warrant a futher study in the field of preventive medicine and health science with respect to efficacy of fermented milk consumption.

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Comparison of Green Color Retention of Zoysiagrass and Cool-season Grass under Multilayer System, USGA System, and Mono-layer System of Sports Field (스포츠용 다단구조, USGA구조 및 약식구조 지반에서 한국잔디 및 한지형 잔디의 녹색기간 비교)

  • Kim, Kyoung-Nam
    • Horticultural Science & Technology
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    • v.34 no.2
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    • pp.342-353
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    • 2016
  • This study was initiated to evaluate green color retention under three different soil systems. Several turfgrasses were evaluated in multi-layer, USGA, and mono-layer systems. Turfgrass entries were comprised of three cultivars of Korean lawngrass (Zoysia japonica Steud.) as warm-season grass (WSG) and three blends and three mixtures of Kentucky bluegrass (KB, Poa pratensis L.), perennial ryegrass (PR, Lolium perenne L.), and tall fescue (TF, Festuca arundinacea Schreb.) as cool-season grass (CSG). Significant differences were observed in visual turf color and green color retention among soil systems and turfgrasses. Both the multi-layer and USGA systems were highly associated with better color ratings and longer color retention, as compared with the mono-layer system. Seasonal variation of visual turf color greatly occurred from late December to early spring. CSG exhibited longer color retention than did WSG. The latter maintained green color for approximately 6 months, regardless of the soil system. Spring green-up of Korean lawngrass occurred from early to middle May, while it underwent discoloration from late October to early November. Among the CSGs green-up occurred between early March and early April and leaf color was maintained until middle December to early February. Therefore, the CSGs were green for 8.5 to 11 months, depending on turfgrass and soil system. The mean period of green color duration across all soil systems was approximately 10-11, 9-10 and 8.5-9.0 months for PR, KB and TF, respectively. As for the CSG mixtures, the greater the proportion of PR, the longer the green color retention, while the higher the proportion of TF, the shorter the color retention. There was greater variation in green color duration among the CSGs than the WSGs. Across soil systems, color retention differences of 2 to 6 days were observed for the Korean lawngrass, but 7 to 36 days for the CSGs. These results demonstrate that green color retention varied greatly according to soil systems and also among turfgrasses. Selections of turfgrass and soil system should be made using a concept-oriented approach, when establishing garden, park, soccer field, golf course and other sports field. Information obtained in this study can be used to select soil systems and turfgrasses based on the expected degree of leaf color retention.

Studies on N-Nitrosamine of Korean Ordinary Soysauce (한국 재래식 간장의 니트로소화합물에 관한 연구)

  • Sung, Nak-Ju;Hwang, Oe-Ja;Lee, Eung-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.17 no.2
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    • pp.125-135
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    • 1988
  • In recent years, the presence of N-nitrosamine, which was produced by the interaction of nitrite and secondary amine, in the fermented foods has been the subject of considerable interest and controversy. In this experiment, the levels of N-nitrosamine such as N-nitrosodimethylamine(NDMA), N-nitrosodiethylamine(NDEA) and N-nitrosodipropylamine(NDPA) in the Korean ordinary soysauce, which were added with ascorbic acid, sorbic acid, and sodium benzoate in the making of it were analyzed by low resolution mass spectrometry, and then the changes of dimethylamine(DMA), nitrate and nitrite nitrogen during the fermentation of it were observed. The contents of DMA nitrogen increased during the fermentation of Korean ordinary soysauce, continuously, but those of DMA nitrogen in the soysauce which had been added with ascorbic acid were inhibited, considerably, until the fermentation of 70days. The levels of nitrate nitrogen during the fermentation of Korean ordinary soysauee decreased, while those of nitrite nitrogen increased. The soysauce which had been incoporated with ascorbic acid in the making of it showed low amounts of nitrite. The concentration of NDMA in the control sample were 2.7 and $8.5{\mu}g/kg$ after the fermentation of 30 and 60 days, respectively, those of NDMA increased during the fermentation of Korean ordinary soysauce, but NDEA and NDPA in all of the soysauce were not detected. The samples were treated with ascorbic acid, sorbic acid, and sodium benzoate in the making of Korean ordinary soysauce were turn out to be effective in preventing the formation of NDMA. Inhibitive actions from food additives as above were, respectively, $82.2{\sim}87.0%$(ascorbic acid), $25.9{\sim}65.4%$(sorbic acid) an $13.2{\sim}63.5%$ (sodium benzoate) in comparison with control sample during the fermentation of Korean ordinary soysauce. NDMA contents were detected below $1.5{\mu}g/kg$ in the soysauce, which food additives were mixed to the pure NaCI in the brewing of it. Free amino acids such as glutamic acid, proline, and histidine were proved to be inhibiting the formation of NDMA during the fermentation of Korean ordinary soysauce. This might be due to the reaction above amino acids and nitrite by Van Slyke reaction.

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Factors Controlling Some Physicochemical Properties of Bentonite (벤토나이트의 물리-화학적 성질을 지배하는 요인분석)

  • 고상모;손병국;송민섭;박성환;이석훈
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.4
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    • pp.259-272
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    • 2002
  • This study was tried to interpret the important major factors controlling some physicochemical properties by comparing mineralogical and physicochemical characteristics such as pH, cation exchange capacity, Methylene Blue adsorption amount, swelling, viscosity, strength (compressional and tensile), and surface area etc. Investigated bentonite samples are five Korean samples from Dusan, Naa, Oksan, Dongyang, and Yeonil deposits and two Japanese bentonites from Tsukinuno and Tomioka deposits which were formed under a similar geological environment of the Tertiary basin. Tsukinuno bentonite is only natural Na-type bentonite and the others are all Ca-type bentonites. Most of the properties are not explained by the montmorillonite content only though the most important factor controlling the physicochemical properties is the montmorillonite content. The layer charge of montmorillonite will strongly control cation exchange capacity and Methylene Blue adsorption. Zeolite bearing bentonites show the strong alkaline character and causes the increase of cation exchange capacity, however decrease swelling, viscosity and strengths. Pyrite bearing bentonites decrease green compressional strength and wet tensile strength. The exchangeable interlayer cations control some physicochemical properties. Na-type bentonite than Ca-type shows more strong alkaline character and much more advanced swelling and viscosity. Also the size and thickness of montmorillonite flakes seem to control some physicochemical properties. Bentonite mainly composed of montmorillonite of very thin and large flakes is characterized by the very high surface area, cation exchange capacity, viscosity, swelling, Methylene Blue adsorption, green compressional strength and wet tensile strength. Domestic Dusan bentonite shows the most excellent physicochemical properties, which is due to the high content(84%) and very well crystallinity of montmorillonite.

Study on Development Effect on Zebrafish Embryo by Alacholr, Butachlor and Fipronil (농약 alacholr, butachlor 및 fipronil이 제브라피쉬 배아 발생에 미치는 영향)

  • Park, Soo Jin;Jeong, Mihye;Paik, Min-Kyoung;Lee, Je-Bong;You, Are-Sun;Hong, SoonSung;Ihm, Yang Bin
    • The Korean Journal of Pesticide Science
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    • v.18 no.1
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    • pp.14-20
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    • 2014
  • This study is aimed to search the possibility of developmental toxicity test using the zebrafish from the pesticide. We selected herbicides alachlor and butachlor, reported for fish toxicity, and insecticide fipronil reported for the high fish toxicity and the honey bee risk among the pesticides with high usability for the examples of the pesticides in this experiment. In this study, we showed those effects on the zebrafish embryo development by exposing different kinds of pesticide with different concentration and exposed time periods. As a result, the rates of hatching and abnormality of the zebrafish embryo after treatments of alachlor were increased in 24-48 hpf group, and the juvenile fishes in every group exposed to $40{\mu}M$ or more of alachlor displayed sever morphological changes such as bent tails, edema and activity failures. In case of the butachlor, the rates of hatching and the abnormality in 24-48 hpf group were higher than the other groups exposed in different time periods. The fatality before hatching was high in $40{\mu}M$ or more of butachlor treatment, and entire zebrafish embryos in 48 hpf group died before hatching. All the living juvenile fishes showed morphological changes as like as the treatment of alachlor. The rate of hatching and the survival of the zebrafish embryo by the fipronil were higher than other pesticides. However, morphological changes such as bent tails were observed from the most of living juvenile fishes. Therefore, the effects of three different pesticides with different concentrations and exposing time periods on the development of zebrafish embryos showed that all the pesticides effects were proportional to the concentration, and exposing time periods may cause the morphological abnormality.