EPMA determined that Fe(Mn)-(oxy)hydroxides and well-crystallized Fe-(oxy)hydroxides and could contain a small amount of As $(0.3-11.0\;wt.\%\;and\;2.1-7.4\;wt.\%\;respectively)$. Amorphous crystalline Fe-(oxy) hydroxide assemblages were identified as the richest in As with $28-36\;wt.\%$. On the ternary $As_2O_5-SO_3-Fe_2O_3$ diagram, these materials were interpreted here as 'scorodite-like'. Dissolved As was attenuated by the adsorption on Fe-(oxy) hydroxides and Fe(Mn)-(oxy) hydroxides and/or the formation of an amorphous Fe-As phase (maybe scorodite: $FeAsO_4\cdot2H_2O$). Leaching tests were performed in order to find out leaching characteristics of As and Fe under acidic conditions. At the initial pHs 3 and 5, As contents dissolved from tailings of the cheongyang mine significantly increased after 7 days due to the oxidation of As-bearing secondary minerals (up to ca. $2.4\%$ of total), while As of Seobo mine-tailing samples was rarely released (ca. $0.0-0.1\%$ of total). Dissolution experiments at an initial pH 1 liberated a higher amount of As (ca. $1.1-4.2\%$ of total for Seobo tailings, $1.5-14.4\%$ of total for Cheongyang tailings). In addition, good correlation between As and Fe in leached solutions with tailings was observed. The kinetic problems could be the important factor which leads to increasing concentrations of As in the runoff water. Release of As from Cheongyang tailings can potentially pose adverse impact to surface and groundwater qualities in the surrounding environment, while precipitation of secondary minerals and the adsorption of As are efficient mechanisms for decreasing the mobilities of As in the surface environment of Seobo mine area.
Sulfoxaflor is a new active ingredient within the sulfoximine insecticide class that acts via a unique interaction with the nicotinic receptor. The MRLs (maximun residue limit) of sulfoxaflor in apple and pear are set at 0.4 mg/kg and that in pepper is set at 0.5 mg/kg. The purpose of this study was to develop an analytical method for the determination of sulfoxaflor residues in agricultural commodities using HPLC-UVD and LC-MS. The analysis of sulfoxaflor was performed by reverse phase-HPLC using an UV detector. Acetone and methanol were used for the extraction and aminopropyl ($NH_2$) cartridge was used for the clean-up in the samples. Recovery experiments were conducted on 7 representative agricultural products to validate the analytical method. The recoveries of the proposed method ranged from 82.8% to 108.2% and relative standard deviations were less than 10%. Finally, LC-MS with selected ion monitoring was also applied to confirm the suspected residues of sulfoxaflor in agricultural commodities.
An isocratic high performance liquid chromatography (HPLC) method for routine analysis of deoxynivalenol in noodles was validated and estimated the measurement uncertainty. Noodles (dried noodle and ramyeon) were analyzed by HPLC-ultraviolet detection using immunoaffinity column for clean-up. The limits of detection (LOD) and quantification (LOQ) were 7.5 ${\mu}g$/kg and 18.8 ${\mu}g$/kg, respectively. The calibration curve showed a good linearity, with correlation coefficients $r^2$ of 0.9999 in the concentration range from 20 to 500 ${\mu}g$/kg. Recoveries and Repeatabilities expressed as coefficients of variation (CV) spiked with 200 and 500 ${\mu}g$/kg were $82{\pm}2.7%$ and $87{\pm}1.3%$% in dried noodle, and $97{\pm}1.6%$ and $91{\pm}12.0%$ in ramyeon, respectively. The uncertainty sources in measurement process were identified as sample weight, final volume, and sample concentration in extraction volume as well as components such as standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. Deoxynivalenol concentration and expanded uncertainty in two matrixes spiked with 200 ${\mu}g$/kg and 500 ${\mu}g$/kg were estimated to be $163.8{\pm}52.1$ and $435.2{\pm}91.6\;{\mu}g$/kg for dried noodle, and $194.3{\pm}33.0$ and $453.2{\pm}91.1\;{\mu}g$/kg for ramyeon using a coverage factor of two which gives a level of statistical confidence with approximately 95%. The most influential component among uncertainty sources was the recovery of matrix, followed by calibration curve.
Park, Gyung Soo;Park, Soung Yun;Lee, Sam Geun;Lee, Yoon
Journal of Wetlands Research
/
v.6
no.1
/
pp.133-147
/
2004
Environmental quality(water and sediment) was analyzed in the tidal flat of Saemangum of Jeonbuk Province, the west coast of Korea, using the 101 sediment samples and 69 water samples collected in September 4~13, 2001. Major water quality parameters with the means of 69 surface water samples are as follows; $25.51{\pm}0.68^{\circ}C$ for water temperature, $29.88{\pm}5.01$ for salinity, $1.40{\pm}0.78mg/L$ for COD, $0.352{\pm}0.417mg/L$ for DIN, and $0.027{\pm}0.023mg/L$ for phosphate, respectively. Higher values were found at the subestuary of Dongjin and Mangyung River, and lower values at the Saemangum embayment and Gomso Bay. There was a significant negative correlation between salinity and the other water quality parameters(p<0.0001) such as COD, nutrients, SS and N/P. This correlation suggested that the major pollution sources be from terrestrial inputs through tributaries in this area. Principal component analysis clearly revealed a spatial variation of water quality; stations with higher values of nutrients and COD located subestuary of tributaries. 14 sediment quality parameters including 8 trace metals were measured using the 101 surface sediment samples. Average values for the parameters are as follows; Al $2.28{\pm}0.92%$, Cd $0.61{\pm}0.27ppm$, Cu $8.95{\pm}4.06ppm$, Fe $1.19{\pm}0.37%$, Mn $182.31{\pm}77.45ppm$, Ni $10.83{\pm}4.97ppm$, Pb $15.20{\pm}4.35ppm$, Zn $41.34{\pm}34.62ppm$, COD $2.68{\pm}1.85mg/g\;dry$, AVS $0.04{\pm}0.08mg/g\;dry$, IL $1.29{\pm}1.08%$, water content $24.11{\pm}4.49%$, TN $0.02{\pm}0.02%$, TC $0.22{\pm}0.30%$. Spatial variations of sediment quality were not clear as water quality. Some higher values were found at the subestuary of Gum River and lower values at the other area. There was a significant positive correlation between the heavy metal concentrations and organic materials within the sediment(p<0.05). Enrichment factors showed the ranges of 1~2 for most of the metals in the sediment except zinc(1~6), indicating no serious exogenous input of heavy metals in the study area. Also, the heavy metal concentrations in the sediment were within the ranges found at the natural marine environments.
Journal of the Korean Society of Food Science and Nutrition
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v.44
no.10
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pp.1504-1509
/
2015
The aim of this study was to investigate a validation method for determination of pectolinarin and pectolinarigenin in fermented Cirsium setidens Nakai. For validation, the specificity, linearity, precision, accuracy, detection limits, and quantification limits of pectolinarin and pectolinarigenin were measured by HPLC. The results show that the detection limits of pectolinarin and pectolinarigenin were $4.25{\mu}g/mL$ and $2.46{\mu}g/mL$, respectively. The recovery rates of pectolinarin and pectolinarigenin were high in the ranges of 99.7~104.0% and 99.7~102.4%, respectively. Inter-day and intra-day precisions of pectolinarin and pectolinarigenin in fermented Cirsium setidens Nakai were 0.9%, 0.5% and 0.5%, 0.2%, respectively. Therefore, application of pectolinarin and pectolinarigenin was validated by an analytical method as a marker compound in Cirsium setidens Nakai.
Infection rates of oyster ovarian parasite, Marteiliodes chungmuensis and productivity of the oyster shellstock infected with the parasite were investigated at the main seed collection areas in the southern coast of Korea where the extreme bad seed collection of oyster occurred in 1992 and 1993 to evaluate the cause of the bad seed collection. Additionally, the bacterial flora of the sea water and oyster lana were examined to identify the shellfish larva pathogenic bacteria like Vibrio sp. and Pseueomonas sp. In August 1992 to September 1993, infection rate of oyster ovarian parasite, M. chungmuensis at Tongyong, Kyongsangnam province, and Yosu, Chollanam province where the bad seed collection occurred, were $11.8\~100\%$ and $14.3\~100\%$, respectively. But the parasite was not detected in the shellstock collected at Daechon, Chungchongnam province. While a virus-like particle was identified in the cytoplasm of the egg infected by the parasite. The parasite infected egg was not able to fertilize completely. Uninfected egg in the gonad contaminated by the parasite could be able to fertilize but showed an abnormal development till D-shaped larva and then, died of necrosis after D-shaped lana. And some lana developed from low lipid content egg could not develop to the spat and died after the early umbo stage. The predominant bacteria in the oyster lana collected at bad seed collection areas were Pseudomonas sp. and Pseudomonas like bacteria and the occupancy rates were $53.3\~87.1\%$.
Kim, Yang-Hyeon;Hong, Su-Myeong;Son, Kyung-Ae;Lee, Ju-Young;Min, Zaw Win;Kwon, Hye-Young;Kim, Taek-Kyum;Kyung, Kee-Sung
The Korean Journal of Pesticide Science
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v.16
no.2
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pp.121-130
/
2012
In analyzing pesticide residue, LLE (liquid liquid extraction) is generally applied as one of the existing methods, but needed quite a lot of organic solvents and analytical apparatuses for the sample pre-treatment. In addition to its long analysis time and complex analytical processes, it is required to develop a more rapid and efficient method at present. In order to establish an economic and simple pesticide residue analytical method, this study carried out a comparative experiment on the existing analytical method with a new sample pre-treatment method named QuEChERS (quick, easy, cheap, effective, rugged and safe), which extracts and refines pesticide components by directly adding solid powder into the sample. Both the two analytical methods showed favorable values of correlation coefficient ($R^2$ > 0.99) of calibration curves. In terms of the detection limit (identification limit), imidacloprid showed 0.02 mg/kg, while the rest of pesticides showed a level around 0.05 mg/kg. The results of this experiment revealed that the recovery of LLE was 92.8-100.9% and the RSD was below 2.5%. On the other hand, the recovery of QuEChERS was 92.2-101.6% and RSD was below 1.9%. As a result of comparing the amount of pesticide residue by the time between the two analytical methods by using Paired t-Test, there was no significant difference between the two analytical methods as the p-value ranged from 0.3148-0.9890. Considering the results of the two methods, the QuEChERS method had similar recovery, compared to the analytical method using the existing LLE, and the analytical time was shortened by about one fourth of that of the existing method. Moreover, since it excludes the use of harmful organic solvents like dichloromethane during the process of extraction, thus leading to protecting experimenters health and remarkably reducing the amount of disused solvents, it is judged as an echo-friendly and economic analytical method.
Purpose: The sentinel lymph node is defined as the first draining node from a primary tumor and reflects the histologic feature of the remainder of the lymphatic basin status. The aim of this study was to evaluate the usefulness of lymphoscintigraphy and intraoperative radioguided gamma probe for identification and removal of sentinel lymph node in breast cancer. Materials and Methods: Lymphoscintigraphy was performed preoperatively in 15 patients with biopsy proven primary breast cancer. Tc-99m antimony sulfide colloid was injected intradermally at four points around the tumor. Imaging acquisition included dynamic imaging, followed by early and late static images at 2 hours. The sentinel lymph node criteria on lymphoscintigraphy is the first node of the highest uptake in early and late static images. We tagged the node emitting the highest activity both in vivo and ex vivo. Histologic study for sentinel and axillary lymph node investigation was done by Hematoxylin-Eosin staining. Results: On lymphoscintigraphy, three of 15 patients had clear lymphatic vessels in dynamic images, and 11 of 15 patients showed sentinel lymph node in early static image and three in late static 2 hours image. Mean detection time of sentinel lymph node on lymphoscintigraphy was $33.5{\pm}48.4$ minutes. The sentinel lymph node localization and removal by lymphoscintigraphy and intraoperative gamma probe were successful in 14 of 15 patients (detection rate: 93.3%). On lymphoscintigraphy, 14 of 15 patients showed $2.47{\pm}2.00$ sentinel lymph nodes. On intraoperative gamma probe, $2.36{\pm}1.96$ sentinel lymph nodes were detected. In 7 patients with positive results of sentinel lymph node metastasis, 5 patients showed positive results of axillary lymph node (sensitivity: 72%) but two did not. In 7 patients with negative results of sentinel lymph node metastasis, all axillary nodes were free of disease (specificity: 100%). Conclusion: Sentinel lymph node biopsy with lymphoscintigraphy and intraoperative gamma probe is a reliable method to predict axillary lymph node metastasis in breast cancer, and unnecessary axillary lymph node dissection can be avoided.
Journal of The Korean Society of Grassland and Forage Science
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v.33
no.1
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pp.21-29
/
2013
The studies were conducted to investigate real condition of mycotoxin contamination in the fields before harvest and by the storages of rice straw used as roughage in Korea. It was found mycotoxin contamination before harvest of rice straw that the rice plants were detected deoxynivalenol at the initial growth, ochratoxin A and deoxynivalenol at the middle growth, and deoxynivalenol and zearalenone at the harvest periods in the fields. Also, the rice plants were contaminated by various fungi such as Fusarium sp., Fusarium proliferatum, Penicillium sp., Gibberella sp., Gibberella zeae, Mucor circinelloides and Aspergillus oryzae. The levels of fungal contamination were $10^{3-4}$ cfu/g at the initial growth, and $10^{4-5}$ cfu/g at the middle growth and harvest periods. All storage types of rice straw were contaminated with zearalenone, deoxynivalenol and ochratoxins A. The samples of rice straw contaminating mycotoxins were account for 3% in bundle rice straw, and 38% in both types of square rice straw and rice round bale silage, respectively. When 105 samples of rice bale silage were analyzed for mycotoxins depending on the regional area, mycotoxin contamination was found in 46% of total samples in Korea. Regional contaminations of mycotoxins were respectively 48, 33, 40, 50 and 57% of samples in Gyeonggi, Gangwon, Chungcheng, Yeongnam and Honam area. Rice round bale silage was contaminated by three kinds of mycotoxins (zearalenone, deoxynivalenol and ochratoxinsA) in the all of area without Chungcheong area where was contaminated zearalenone and deoxynivalenol. Ochratoxins A, deoxynivalenol and zearalenone were respectively determinated with the average levels of 2.6, 413 and $338{\mu}g/kg$ in rice round bale silage for the overall area, even if it was some difference depending on each regional area. Therefore, the above results clearly show that the rice straws were exposed to the contamination by mycotoxin and mycotoxigenic fungi before harvest in the fields, and mycotoxin contamination was not dependent on the regional area or the storage types such as bundle rice straw, square rice straw and rice round bale silage.
The aim of this study was to determine the methylmercury (MeHg) levels in abyssal fish species. The MeHg in the fishes was extracted with hydrochloric acid and toluene and then purified using an L-cysteine solution. The extract was analyzed with a gas chromatography-electron capture detector (GC-${\mu}ECD$) with a thermon Hg-capillary column. The detection limit and the recovery of the method were 0.002 and 84.2-98.5% (mean, 93.4%), respectively. The MeHg content in 492 abyssal fishes ranged from 0.037 to 2.009 mg/kg. The levels of MeHg [range, mg/kg (mean)] were significantly dependent on fish species and presented as the following; 0.157-2.009 (0.546) in Scalloped hammerhead shark, 0.211-0.878 (0.501) in Blue shark, 0.121-0.993 (0.482) in Spiny dogfish, 0.243-0.658 (0.397) in Salmon shark, 0.074-1.958 (0.353) in Blacktip shark, 0.038-0.807 (0.302) in Southern hake, 0.099-0.511 (0.300) in Scorpion fish, and 0.037-0.133 (0.067) in Ling. The monitoring results showed that the estimated weekly intake of MeHg from sharks, Southern hake, and Ling were lower than the provisional tolerable weekly intake recommended by the Joint FAO/WHO expert committee on food additives.
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