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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.

Study on the Technological System of the Cooperative Cultivation of Paddy Rice in Korea (수도집단재배의 기술체계에 관한 연구)

  • Min-Shin Cho
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.8 no.1
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    • pp.129-177
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    • 1970
  • For the purpose of establishing the systematized technical scheme of the cooperative rice cultivation which has most significant impact to improve rice productivity and the farm management, the author have studied the cultivation practices, and the variation of rice growth and yield between the cooperative rice cultivation and the individual rice cultivation at random selected 18 paddy fields. The author also have investigated through comparative method on the cultivation practices, management, organization and operation scheme of the two different rice cultivation methods at 460 paddy fields. The economic feasibility has been ana lysed and added in this report. The results obtained from this study are summarized as follows; 1. In the nursery, the average amount of fertilizer application, especially, phosphate and potassium, and the frequency of chemicals spray for the disease, insect and pest control at the cooperative rice cultivation are significantly higher than those of the individual rice cultivation. 2. The cultivation techniques of the cooperative rice farming after the transplanting can be characterized by a) the earlier transplanting of rice, b) the denser hills per unit area and the lesser number of seedlings per hill, c) the application of larger quantities of fertilizer including nitrogen, phosphate and potassium, d) more divided application of fertilizers, split doses of the nitrogen and potassium, e) the increased frequencies of the chemicals spray for the prevention of disease, insect and pest damages. 3. The rate of lodging in the cooperative rice cultivation was slightly higher than that of the individual rice cultivation, however, the losses of rice yield owing to the occurrence of rice stem borer and grass leaf roller in the cooperative rice cultivation were lower than that of the individual rice cultivation. 4. The culm length, panicle length, straw weight and grain-straw ratio are respectively higher at the cooperative rice cultivation, moreover, the higher variation of the above factors due to different localities of the paddy fields found at the individual rice cultivation. 5. The number of panicles, number of flowers per panicle and the weight of 1, 000 grains, those contributing components to the rice yield were significantly greater in the cooperative rice cultivation, however, not clear difference in the maturing rate was observed. The variation coefficient of the yield component in the cooperative cultivation showed lower than that or the individual rice cultivation. 6. The average yield of brown rice per 10 are in the cooperative rice cultivation obtained 459.0 kilograms while that of the individual rice cultivation brought 374.8 kilograms. The yield of brown rice in the cooperative rice cultivation increased 84.2 kilogram per 10 are over the individual rice cultivation. With lower variation coefficient of the brown rice yield in the cooperative rice cultivation, it can be said that uniformed higher yield could be obtained through the cooperative rice cultivation. 7. Highly significant positive correlations shown between the seeding date and the number of flowers per panicle, the chemical spray and the number of flowers per panicle, the transplanting date and the number of flowers per panicle, phosphate application and yield, potassium application and maturing rate, the split application of fertilizers and yield. Whilst the significant negative correlation was shown between the transplanting date and the maturing rate 8. The results of investigation from 480 paddy fields obtained through comparative method on the following items are identical in general with those obtained at 18 paddy fields: Application of fertilizers, chemical spray for the control of disease, insects and pests both in the nursery and the paddy field, transplanting date, transplanting density, split application of fertilizers and yield n the paddy fields. a) The number of rice varieties used in the cooperative rice cultivation were 13 varieties while the individual rice cultivation used 47 varieties. b) The cooperative rice cultivation has more successfully adopted improved cultivation techniques such as the practice of seed disinfection, adoption of recommended seeding amount, fall ploughing, application of red soil, introduction of power tillers, the rectangular-type transplanting, midsummer drainage and the periodical irrigation. 9. The following results were also obtained from the same investigation and they are: a) In the cooperative rice cultivation, the greater part of the important practices have been carried out through cooperative operation including seed disinfection, ploughing, application of red soil and compost, the control of disease, insects and pests, harvest, threshing and transportation of the products. b) The labor input to the nursery bed and water control in the cooperative rice cultivation was less than that of the individual rice cultivation while the higher rate of labor input was resulted in the red soil and compost application. 10. From the investigation on the organization and operation scheme of the cooperative rice cultivation, the following results were obtained: a) The size of cooperative rice cultivation farm was varied from. 3 ha to 7 ha and 5 ha farm. occupied 55.9 percent of the total farms. And a single cooperative farm was consisted of 10 to 20 plots of paddies. b) The educational back ground of the staff members involved in the cooperative rice cultivation was superior than that of the individual rice cultivation. c) All of the farmers who participated to the questionaires have responded that the cooperative rice cultivation could promise the increased rice yield mainly through the introduction of the improved method of fertilizer application and the effective control of diseases, insects and pests damages. And the majority of farmers were also in the opinion that preparation of the materials and labor input can be timely carried out and the labor requirement for the rice cultivation possibly be saved through the cooperative rice cultivation. d) The farmers who have expressed their wishes to continue and to make further development of the cooperative rice cultivation was 74.5 percent of total farmers participated to the questionaires. 11. From the analysis of economical feasibility on the two different methods of cultivation, the following results were obtained: a) The value of operation cost for the compost, chemical fertilizers, agricultural chemicals and labor input in the cooperative rice cultivation was respectively higher by 335 won, 199 won, 288 won and 303 won over the individual rice cultivation. However, the other production costs showed no distinct differences between the two cultivation methods. b) Although the total value of expenses for the fertilizers, agricultural chemicals, labor input and etc. in the cooperative rice cultivation were approximately doubled to the amount of the individual rice cultivation, the net income, substracted operation costs from the gross income, was obtained 24, 302 won in the cooperative rice cultivation and 20, 168 won was obtained from the individual rice cultivation. Thereby, it can be said that net income from the cooperative rice cultivation increased 4, 134 won over the individual rice cultivation. It was revealed in this study that the cooperative rice cultivation has not only contributed to increment of the farm income through higher yield but also showed as an effective means to introduce highly improved cultivation techniques to the farmers. It may also be concluded, therefore, the cooperative rice cultivation shall continuously renovate the rice production process of the farmers.

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Variation of Genus Ilex in Korea and their Ornamental Values (Ilex속(屬) 수목(樹木)의 유전변이(遺傳變異)의 분석(分析)과 조경학적(造景學的) 이용가치(利用價値)의 조사(調査) 연구(硏究))

  • Yim, Kyong Bin
    • Journal of Korean Society of Forest Science
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    • v.42 no.1
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    • pp.1-38
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    • 1979
  • The woody species of Genus Ilex which are endemic to Korea are distributed on limited area due to solely temperature factor. There is some differences according to species, however in general, the evergreen Ilex are found along southern coastal area of Korean Peninsula and near islands where the cold index does not exceed $-5^{\circ}C$. But Ilex macropoda and the variety, only deciduous ones, are grown in temperate zone of the peninsula and some islands. The list of Ilex species of Korea are as follows. Ilex cornuta Lindley et Pax., I. crenata Thunb. var. microphylla Max., I. crenata Thunb., I. rotunda Thunb., I. macropoda Miq., I. macropoda Miq. var. pseudo-macropoda Loensner, I. integra Thunb. The author surveyed the populations of Ilex species as many as possible and data of some characters such as leaf shape, spine, fruit shape, stomata density, sex ratio in natural communities, etc. are collected. Almost all the Ilex species in Korea show sporadic distribution. This means quite small sized populations isolate distantly each other eliminating the change of gene exchange in between. Particularly Ilex conuta and I. crenata show the morphological differentiation among populations as well as significant individual variation within a population. These were true with such characteristics, leaf shape, leaf dimension, leaf margin, fruit shape, spine, and stomata density. The founded are that the fruit length and the stomata density counted on the beneath surface of leaves of Ilex cornuta increased with the decrease of latitude. These are naturally closely related with the cold index values. The table shown below indicates the correlation between mean stomata density per $0.3642mm^2$ and cold index values. These relation however were not observed on Ilex crenata. The most dominated natured in relation to individual variation were outline of leaf, the number of marginal spine, the shape of leaf cross section and the degree of luster of the upper leaf surface. As shown in photos 5~7, these variations are agreed at a glance. There are reports that the development of marginal spines in some Ilex species is associated with the juvenility and topophysis. In present study, these two factors were neglected because of the intended sampling procedure. Of Ilex rotunda, population difference with the characteristics of leaf length is recognized but not for leaf width, petiole length, and fruit size. However, individual variations within a population were significantly large. In case of Ilex integra, only individual differences within population were calculated statistically for such characteristics as leaf length, leaf width, and petiole length. As to natural population, the sex ratio was 1:2 (female to male) for Ilex cornuta, and 1:1 for Ilex crenata. The tendency of more male than female in I. cornuta was agreed to other observations. Preparing the tip cutting of length 10cm, and treating with IBA, then attaching earth ball to the cut end, very successful rooting percentages were obtained. Asexual propagation has the advantages of maintaining the heterozygosity of existing varieties and overcoming the difficulties of delayed seed germination frequently encountered with Ilex species. Considering a great deal of variation in morphological traits, a good possibility of selection breeding for decorative and ornamental purposes exists. At present, these evergreen Ilex are ignored by local people as nuisance weedy shrubs. So the proper protection measures should promptly be taken.

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Studies on the Method of Ground Vegetation Establishment of Denuded Forest Land in the Mudstone Region - The Characteristics of Mudstone and Speeded-up Reforestation - (니암지대황폐림지(泥岩地帶荒廢林地)의 지피식생(地被植生) 조성방법(造成方法)에 관(關)한 연구(硏究) - 니암특성((泥岩特性)과 조기녹화(早期綠化) -)

  • Chung, In Koo
    • Journal of Korean Society of Forest Science
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    • v.19 no.1
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    • pp.1-23
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    • 1973
  • The results of ground vegetation experiment conducted at completely denuded forestland in the mudstone region are summerized as follows: On the reaults of soiling quantity the effect of soiling was observed where depth of soiling over 10 cm was practiced, and a plot where treated with 15cm soiling and without fertilizer showed poor growth and it was even worser than the plot where soiling was practiced only 1 cm in thikness but applied adequate amount of fertilizers. The depth of slits between 30cm and 40cm showed no significant difference in the effect. A plot where covered with vegetation bag showed somewhat better results in seed loss and early growth but no differences observed in the fall result over the none covered plot. And then, it is recommendable to have soiling over 10cm in thikness with slit of 30cm and 30cm in depth and to apply 30 gram of fertilizer (22;22:11, 50 gram) per slit. On various soiling materials trial there were no striking differences in the effect of soiling between weathered granite soil, wheathered tuffs soil and weathered mudstone soil. In the treatment with various green materials, a plot treated with straw mat showed a significant difference at 1 percent. The results show that weathered mudstone soil is effective to use as soiling materials and straw mat treatment was better. On forest fertilization trial, in the mudstone region where red and black pine trees already existing at a rate of 2,000-3,000 trees per hectare had applied 110kg of compound fertilizers (9:12:3 and 22:22:11) per hectare basis in terms of plant nutrient. As a result, the difference in effect between the compound fertilizers was not found however the leaf color and leaf length of the fertilizer added plot showed darker and longer at 30 percent over the no fertilizer received plot. Compound fertilizers, 14:37:12 and 9:12:3 were applied to alder trees at a rate of 20 gram and 40 gram per tree in terms of plant nutrient and a remarkable growth accelerantion was observed where 40 grams of plant nutrient applied. The effect difference between the compound fertilizers was not found. On investigation of tree root elongation, forty years old red pine trees showed only 15cm tap root elongation through mudstone while black pine had 23 cm tap root elongation. The total length of supporting root elongtion of red and black pines showed 20 and 13 meters, respectively. The tap roots of Black locusts were not able to elongate through mudstone, however, the supporting roots tended to develop to the underneath of pine tree where some moisture content is available. Black locusts And grown on the residual soil of mudstone normally die between 8 to 10 years. The red pine trees show flat in tree shape while black pine had triangle in the shape. With the results it can be said that in an artificial reforestation in denuded forest land of the mudstone region the adequate slit and enough amount of fertiliizer application must be provided for the succesful performance of the program. On integrated experimental results of 1972. for the establishment of ground vegetation on the completely denuded forest land in mudstone region, soiling could be effectively practiced with weathered mudstone soil and it would not specially necessiate to have either weathered granite or tuffssoil for the soiling. And the soiling depth should be more than 10 cm in thickness. Among green materials used the straw mat proved to be the most effective reatment. Three major factors which enable to establish ground vegetation by the shortest period of time: A. Physical improvement of soil is necessary to breakdown of the horizontal cracks sushas Slit, contour line plot, seeding hole and etc., and soiling with weathered mudstone soil. B. Chemical improvement of soil: is needed sufficient amount of fertilizer application 300~400kg ha, $N+P_2O_5+K_2O$), and increased production of ground covering and expedite resolution of the vegetation (ground vegetation, fallen leaves and twigs). C. Complete establishment of the basic structure for the erosion control (Prevention of surface soil erosion)

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