Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO4 and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R2) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.
Kim, Kyung-Min;Jang, Taek-Gyun;Kim, Young-Ho;Oh, Sang-Huyb;Lee, Sang-Hak
Analytical Science and Technology
/
v.24
no.4
/
pp.243-248
/
2011
A selective determination method of mercury (II) ion in aqueous solution by luminol-based chemiluminescence system (luminol CL system) has been developed. Determination of metal ions such as copper (II), iron (III), chromium (III) ion in solution by the luminol CL system using its catalytic role in the reaction of luminol and hydrogen peroxide has been reported by several groups. In this study, the catalytic activity of mercury (II) ion in the reaction of luminol and hydrogen peroxide was observed by the enhanced CL intensity of the luminol CL system. Based on this phenomenon, experimental conditions of the luminol CL system were investigated and optimized to determine mercury (II) ion in aqueous solution. While mercury (II) ion in mixed sample solution containing mercury (I) and (II) ions highly enhanced the CL intensity of the luminol CL system, the mercury (I) ion could not enhanced the CL intensity. Thus selective determination of the mercury (II) ions in a mixture containing mercury (I) and (II) ions could be achieved. Each concentration of mercury (I) and (II) ions in aqueous solution can be obtained from the results of the CL method that give the concentration of only mercury (II) ion and the inductively coupled plasma (ICP) method that give the total concentration of mercury ions. On the optimized conditions, the calibration curve of mercury (II) ion was linear over the range from $1.25{\times}10^{-5}$ to $2.50{\times}10^{-3}M$ with correlation coefficient of 0.991. The detection limit of mercury (II) ion in aqueous solution was calculated to be $1.25{\times}10^{-7}M$.
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.
Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
Korean Journal of Food Science and Technology
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v.44
no.3
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pp.263-268
/
2012
Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.
Purpose: Thallous-201 chloride produced at Korea Cancer Center Hospital(KCCH) is used in detecting cardiovascular disease and cancer. Thallium impurity can cause emesis, catharsis and nausea, so the presence of thallium and other metal impurities should be determined. According to USP and KP, their amounts must be less than 2 ppm in thallium and 5 ppm in total. In this study, the detection method of trace amounts of metal impurities in $[^{201}Tl]$TICI injection with polarography was optimized without environmental contamination. Materials and Methods: For the detection of metal impurities, Osteryoung Square Wave Stripping Voltammetry method was used in Bio-Analytical System (BAS) 50W polarograph. The voltammetry was composed of Dropping Mercury Electrode (DME) as a working electrode, Ag/AgCl as a reference electrode and Pt wire as a counter electrode. Square wave stripping method, which makes use of formation and deformation of amalgam, was adopted to determine the metal impurities, and pH 7 phosphate buffer was used as supporting electrolyte. Results: Tl, Cu and Pb in thallous-201 chloride solution were detected by scanning from 300 mV to -800 mV Calibration curves were made by using $TINO_3,\;CuSO_4\;and\;Pb(NO_3){_2}$ as standard solutions. Tl was confirmed at -450 mV peak potential and Cu at -50 mV Less than 2 ppm of Tl and Cu was detected and Pb was not detected in KCCH-produced thallous-201 chloride injection. Conclusion: Detection limit of thallium and copper is approximately 50 ppb with this method. As a result of this experiment, thallium and other metal impurities in thallous-201 chloride injection, produced at Korea Cancer Center Hospital, are in the regulation of USP and KP Polarograph could be applied for the determination of metal impurities in the quality control of radiopharmaceuticals conveniently without environmental contamination.
Journal of Korean Society of Coastal and Ocean Engineers
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v.31
no.3
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pp.158-169
/
2019
A probabilistic model that can predict the residual useful lifetime of structure is formulated by using the gamma process which is one of the stochastic processes. The formulated stochastic model can take into account both the sampling uncertainty associated with damages measured up to now and the temporal uncertainty of cumulative damage over time. A method estimating several parameters of stochastic model is additionally proposed by introducing of the least square method and the method of moments, so that the age of a structure, the operational environment, and the evolution of damage with time can be considered. Some features related to the residual useful lifetime are firstly investigated into through the sensitivity analysis on parameters under a simple setting of single damage data measured at the current age. The stochastic model are then applied to the rubble-mound breakwater straightforwardly. The parameters of gamma process can be estimated for several experimental data on the damage processes of armor rocks of rubble-mound breakwater. The expected damage levels over time, which are numerically simulated with the estimated parameters, are in very good agreement with those from the flume testing. It has been found from various numerical calculations that the probabilities exceeding the failure limit are converged to the constraint that the model must be satisfied after lasting for a long time from now. Meanwhile, the expected residual useful lifetimes evaluated from the failure probabilities are seen to be different with respect to the behavior of damage history. As the coefficient of variation of cumulative damage is becoming large, in particular, it has been shown that the expected residual useful lifetimes have significant discrepancies from those of the deterministic regression model. This is mainly due to the effect of sampling and temporal uncertainties associated with damage, by which the first time to failure tends to be widely distributed. Therefore, the stochastic model presented in this paper for predicting the residual useful lifetime of structure can properly implement the probabilistic assessment on current damage state of structure as well as take account of the temporal uncertainty of future cumulative damage.
Lee, Ji Hyeon;Jung, Sang Hyung;Kim, Jun Ho;Min, Eun Joo;Yeo, Un Yeong;Kim, Jong Woo
Journal of Intelligence and Information Systems
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v.26
no.1
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pp.97-117
/
2020
Product evaluation criteria is an indicator describing attributes or values of products, which enable users or manufacturers measure and understand the products. When companies analyze their products or compare them with competitors, appropriate criteria must be selected for objective evaluation. The criteria should show the features of products that consumers considered when they purchased, used and evaluated the products. However, current evaluation criteria do not reflect different consumers' opinion from product to product. Previous studies tried to used online reviews from e-commerce sites that reflect consumer opinions to extract the features and topics of products and use them as evaluation criteria. However, there is still a limit that they produce irrelevant criteria to products due to extracted or improper words are not refined. To overcome this limitation, this research suggests LDA-k-NN model which extracts possible criteria words from online reviews by using LDA and refines them with k-nearest neighbor. Proposed approach starts with preparation phase, which is constructed with 6 steps. At first, it collects review data from e-commerce websites. Most e-commerce websites classify their selling items by high-level, middle-level, and low-level categories. Review data for preparation phase are gathered from each middle-level category and collapsed later, which is to present single high-level category. Next, nouns, adjectives, adverbs, and verbs are extracted from reviews by getting part of speech information using morpheme analysis module. After preprocessing, words per each topic from review are shown with LDA and only nouns in topic words are chosen as potential words for criteria. Then, words are tagged based on possibility of criteria for each middle-level category. Next, every tagged word is vectorized by pre-trained word embedding model. Finally, k-nearest neighbor case-based approach is used to classify each word with tags. After setting up preparation phase, criteria extraction phase is conducted with low-level categories. This phase starts with crawling reviews in the corresponding low-level category. Same preprocessing as preparation phase is conducted using morpheme analysis module and LDA. Possible criteria words are extracted by getting nouns from the data and vectorized by pre-trained word embedding model. Finally, evaluation criteria are extracted by refining possible criteria words using k-nearest neighbor approach and reference proportion of each word in the words set. To evaluate the performance of the proposed model, an experiment was conducted with review on '11st', one of the biggest e-commerce companies in Korea. Review data were from 'Electronics/Digital' section, one of high-level categories in 11st. For performance evaluation of suggested model, three other models were used for comparing with the suggested model; actual criteria of 11st, a model that extracts nouns by morpheme analysis module and refines them according to word frequency, and a model that extracts nouns from LDA topics and refines them by word frequency. The performance evaluation was set to predict evaluation criteria of 10 low-level categories with the suggested model and 3 models above. Criteria words extracted from each model were combined into a single words set and it was used for survey questionnaires. In the survey, respondents chose every item they consider as appropriate criteria for each category. Each model got its score when chosen words were extracted from that model. The suggested model had higher scores than other models in 8 out of 10 low-level categories. By conducting paired t-tests on scores of each model, we confirmed that the suggested model shows better performance in 26 tests out of 30. In addition, the suggested model was the best model in terms of accuracy. This research proposes evaluation criteria extracting method that combines topic extraction using LDA and refinement with k-nearest neighbor approach. This method overcomes the limits of previous dictionary-based models and frequency-based refinement models. This study can contribute to improve review analysis for deriving business insights in e-commerce market.
Kim, Yeong-Tae;Kim, Gui-Young;Jeon, Kyeong-Am;Lee, Dae-In;Yu, Jun;Kim, Hee-Jung;Kim, In-Chul;Eom, Ki-Hyuk
Journal of the Korean Society of Marine Environment & Safety
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v.19
no.2
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pp.119-128
/
2013
Since the early 2000s, demand for coastal dredging projects have been significantly increased, and the dredged sediments have showed the continuing marked increases through the multiple projects with other coastal development and constructions. As significant or potential degradation of marine environment has been mounting, we checked the current situation of marine environmental impact assessment through marine water and sediment qualities in relation with dredging projects of the sea area utilization consultation statements submitted in 2011. While analysis percentages of the general items were usually higher, harmful components such as metals revealed wide variation of analysis percentages. In the event of analysis of metals, the pre-treatment process (full digestion) and analysis method were not properly implemented in accordance with the guidelines for preparation of consultation statements. Although not specified in the guidelines, verification procedures (tests of recovery efficiency and detection limit) to secure the reliability were almost ignored. As a result, most of developers did conduct poor marine environmental impact assessment on coastal dredging and related projects. We suggested that the responsible government authority should establish new detailed guidelines on the sea area utilization consultation for more strict evaluation and diagnosis of marine environment and distinctly request the developer to obey the guidelines by complementing the system of the sea area utilization consultation.
Journal of the Korean Society of Food Science and Nutrition
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v.46
no.9
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pp.1097-1105
/
2017
This study examined how much chicken meat was in sausage made with pork. Both real-time polymerase chain reaction (PCR) and internal standard addition were used. Fifty ng of chicken DNA was added to the sausages as an internal standard. The addition of standard DNA increased the amplification efficiency of PCR and confirmed the possibility of quantitative analysis. A QIAamp DNA Micro Kit was used to improve the DNA recovery and amplification efficiency. The density of template DNA and primer were suitable for $3.0{\sim}5.0{\mu}L$ and $0.5{\mu}L$, respectively. Each DNA of pig and chicken was diluted in 10-fold from steps 50 ng to 0.05 ng. The detection limit of both pig and chicken meat was more than 0.05 ng and the correlation coefficient of the standard curve was at least 0.98. The result of the quantitative analysis after heat treatment of 3 samples of pigs and chickens mixed at 70:30 showed a 5.7% difference (64.3:35.7) between the expected value and measured value. The quantitative value was changed by affecting the DNA according to the heat treatment ($70^{\circ}C$, 10 min). An analysis of the pork and chicken content in sausages showed that it was difficult to detect chicken meat and the quantitative value of DNA according to the Ct value was very low. On the other hand, when adding standard material (50 ng of chicken DNA) to the sausages, the Ct value decreased gradually with increasing chicken mixing ratio. Thus, the mixing ratio of chicken in sausages could be estimated.
Kwon, Oh Jun;Hur, Jae;Lee, Han Wool;Kim, Joo Yeon;Park, Min Soo;Roo, Dong Ook;Kang, Chun Goo;Kim, Jae Sam
The Korean Journal of Nuclear Medicine Technology
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v.19
no.1
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pp.30-36
/
2015
Purpose Whole body bone scan, which makes up a largest percentage of nuclear medicine tests, has high sensitivity and resolution about bone lesion like osteomyelitis, fracture and the early detection of primary cancer. However, any standard for valuation has not yet been created except minimum factor. Therefore, in this study, we will analysis the method which show a quantitative evaluation index in whole body bone scan. Materials and Methods This study is conducted among 30 call patients, who visited the hospital from April to September 2014 with no special point of view about bone lesion, using GE INFINIA equipment. Enumerated data is measured mainly with patient's whole body count and lumbar vertabrae, and the things which include CNR (Contrast to Noise ratio), SNR (Signal to Noise ratio) are calculated according to the mean value signal and standard deviation of each lumbar vertabrae. In addition, the numerical value with the abdominal thickness is compared to each value by the change of scan speed and tissue equivalent material throughout the phantom examination, and compared with 1hours deleyed value. Completely, on the scale of ten, 2 reading doctors and 5 skilled radiologists with 5-years experience analysis the correlation between visual analysis with blind test and quantitative calculation. Results The whole body count and interest region count of patients have no significant correlation with visual analysis value throughout the blind test(P<0.05). There is definite correlation among CNR and SNR. In phantom examination, Value of the change was caused by the thickness of the abdomen and the scan speed. And The poor value of the image in the subject as a delay test patient could be confirmed that the increase tendency. Conclusion Now, a standard for valuation has not been created in whole body bone scan except minimum factor. In this study, we can verify the significant correlation with blind test using CNR and SNR and also assure that the scan speed is a important factor to influence the imagine quality from the value. It is possible to be some limit depending on the physiology function and fluid intake of patient even if we progress the evaluation in same condition include same injection amount, same scan speed and so on. However, that we prove the significant evaluation index by presenting quantitative calculation objectively could be considered academic value.
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