BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine HCl and heated at $60^{\circ}C$ in microwave for 20 min. Methylmercury in $50{\mu}L$ of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine HCl + 0.1% L-cysteine mobile phase at $25^{\circ}C$. The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient($r^2$) for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and $0.45{\mu}g/kg$ respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.
Kim, Hyun Tae;Han, Won Young;Lee, Byung Won;Ko, Jong Min;Lee, Yeong Hoon;Baek, In Youl;Yun, Hong Tai;Ha, Tae Joung;Choi, Man Soo;Kang, Beom Kyu;Kim, Hyun Yeong;Seo, Jeong Hyun;Kim, Hong Sik;Shin, Sang Ouk;Oh, Jae Hyun;Kwak, Do Yeon;Seo, Min Jeong;Song, Yoon Ho;Jang, Eun Kyu;Yun, Geon Sik;Kang, Yeong Sik;Lee, Ji Yun;Shin, Jeong Ho;Choi, Kyu Hwan;Kim, Dong Kwan;Yang, Woo Sam
Korean Journal of Breeding Science
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v.51
no.4
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pp.496-503
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2019
The soybean cultivar, 'Saegeum', has been developed for preparing soy-paste and tofu. The soybean cultivars 'Daepung' and 'SS98207-3SSD-168' were crossed in 2003 to obtain 'Saegeum'. Single seed descent method was used to advance the generation from F3 to F5, and the plant lines with promising traits were selected from F6 to F7 by pedigree method. The preliminary yield (PYT) and advanced yield trials (AYT) were conducted from 2009 to 2010, and the regional yield trial (RYT) was conducted in 12 regions between 2011 and 2013. The morphological characteristics of 'Saegeum' were as follows: determinate plant type, white flower, tawny pubescence color, and brown pod color. Flowering and maturity dates were August 2, XXXX and October 17, XXXX, respectively. Plant height, first pod height, number of nodes, number of branches, and number of pods were 79 cm, 18 cm, 16, 2.3, and 44, respectively. The seed characteristics of 'Saegeum' were as follows: yellow spherical shape, yellow hilum, and the 100-seed weight was 25.4 g. 'Saegeum' was resistant to bacterial pustule and SMV in the field test, and its lodging resistance was mildly strong, whereas its shattering resistance was excellent. The ability of this cultivar to be processed into tofu, soybean malt, and other fermented products was comparable with that of 'Daewonkong'. The yield of 'Saegeum' in the adaptable regions was 3.02 ton ha-1. Thus, 'Saegeum' is adaptable to mechanized harvesting because of its high first pod height, as well as lodging and shattering resistance. (Registration number: 5929)
An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.
Ku, Ja-Hwan;Han, Ouk-kyu;Oh, Young-Jin;Park, Tae-Il;Kim, Dae-Wook;Kim, Byung-Joo;Park, Myoung Ryoul;Ra, Kyung-Yoon
Journal of The Korean Society of Grassland and Forage Science
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v.40
no.4
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pp.209-215
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2020
A winter forage tetraploid rye (Secale cereale L.) cultivar, 'Daegokgreen', was developed at the Department of Central Area Crop Science, NICS, RDA in 2016. The mutant line 'CG11003-8-B', which was induced from rye cultivar 'Gogu' (diploid) by colchicine treatment, was selected for its excellent agronomic performance and was placed in preliminary yield trials for one year, 2013. The line was designated "Homil59" and was tested for regional yield trials at the four locations in Korea from 2014 to 2016. Finally, the new cultivar was named as the 'Daegokgreen' (grant number 8274). The leaf of cultivar 'Daegokgreen' is wide, long and dark-green color. The cultivar also has a big-size grain with light-brown color. The heading date of cultivar 'Daegokgreen' was April 17 which was 2 days later than that of check cultivar 'Gogu'. The tolerance to cold and wet injury, and resistance to powdery mildew and leaf rust of the new cultivar were similar to those of the check cultivar but the resistance to the lodging of the new cultivar was stronger than that of the check. The average roughage fresh and dry matter yield of the new cultivar after 10 days from heading were 37.0 and 7.7 MT ha-1, respectively, which were similar to those (38.4 and 8.0 MT ha-1) of the check cultivar. The roughage quality of 'Daegokgreen' was higher in crude protein content (8.9%) than that of the check cultivar (7.9%), while was similar to the check in total digestible nutrients (56.9%). This cultivar is recommended for fall sowing forage crops at all of crop cultivation areas in Korea.
This study was performed to develop a suitable nutrient solution for standard rose substrate culture in a closed hydroponic system. 1/4, 1/2, 2/3 and 1 strength of the nutrient solution made by Japan National Institute of Vegetable and Tea Science (JNIVT) were supplied. The photosynthesis rate, quality and growth of cut flower were higher in the 1/2 and 2/3 strength of nutrient solution during high and low temperature period. Based on the above results, optimum nutrient solutions (UOS) were composed by nutrientwater (n/w) absorption ratio with 1/2S ($NO_{3^-}N$ 6.8, $NH_{4^-}N$ 0.7, $PO_{4^-}P$ 2.0, K 3.8, Ca 3.0, Mg 1.2, $SO_{4^-}S$$1.2me{\cdot}L^{-1}$) at high temperature season and 2/3($NO_{3^-}N$ 9.7, $NH_{4^-}N$ 0.8, $PO_{4^-}P$ 2.2, K 5.0, Ca 3.9, Mg 1.5, $SO_{4^-}S$$1.5me{\cdot}L^{-1}$) at low temperature season. The results of suitability examination showed that the EC level in newly composed nutrient solution (UOS) was more stable than other nutrient solutions due to its large amount of calcium and potassium. The growth of cut flower cultivated with UOS was higher than those of other nutrient solutions. Especially, the yield of cut flowers in UOS nutrient solution increased 1.4 times than that of other nutrient solution treatments. Consequently, the new nutrient solution investigated in this experiment was suitable for rose cultivation in a closed hydroponic system.
The experiment was conducted to investigate the nutrition absorption pattern in the growth stages and develope the optimal nutrient solution hydroponically grown the tomato in closed substrate culture system with the nutrient solution of National Horticultural Research Station in Japan into 1/2S, 1 S, and 2S. When plant was grown in 1/2 S, the growth and yield were high and the pH and EC in the rooting zone were stable. Suitable composition of nutrient solution for tomato was $NO_3-N$ 7.1, $PO_{4}$-P 2.1, K 4.0, Ca 3.1, Mg 1.2, and $SO_{4}-S\;1.2\;me{\cdot}L^{-1}$ in the early growth stage and $NO_3-N$ 6.5, $PO_4-P$ 2.3, K 3.4, Ca 3.1, Mg 1.1, and $SO_4-S\;1.1\;me{\cdot}L^{-1}$ in the late growth stage by calculating a rate of nutrient and water uptake. To estimate the suitability for the nutrient solution of tomato in a development of optimum nutrient solution of tomato developed by Wonkwang university in korea (WU), plant was grown in perlite substrate supplied with different solution and strengths(S) by research station for greenhouse vegetable and floricultuin in the Netherlands (Proefstation voor tuinbouw onder glas te Naaldwijk; PTG) of 1/2 S, 1 S and 2 S, respectively, The growth was good at the PTG and WU of 2 S in early growth stage, and at the WU 2S in late growth stage. The highest yield of tomato obtained in the WU of 2 S, although blossom-end rot was appeared in all treatments. pH and EC in root zone of WU of 2 S were stable during the early and late growth stage. Therefore when plant was grown in WU of 2 S, N and P content in the nutrient solution need to low, according N and P content of their leaves were high in WU of 2 S.
Mi-Hui Son;Jae-Kwan Kim;You-Jin Lee;Ji-Eun Kim;Eun-Jin Baek;Byeong-Tae Kim;Seong-Nam Lee;Myoung-Ki Park;Yong-Bae Park
Journal of Food Hygiene and Safety
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v.38
no.4
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pp.211-216
/
2023
A total of 100 commercially available olive oil products were analyzed for 179 pesticide residues using gas chromatography-tandem mass spectrometry (GC/MS/MS). The olive oil samples were mixed with organic solvents, centrifuged and frozen to remove fat, and pesticide residues were analyzed using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method. The determination coefficient (R2) of the analysis method used in this study was ≥0.998. The detection limit of the method ranged 0.004-0.006 mg/kg and its quantitative limit ranged 0.012-0.017 mg/kg. The recovery rate (n=5) measured at the level ranging 0.01-0.02, 0.1, and 0.5 mg/kg ranged 66.8-119.5%. The relative standard deviation (RSD) was determined to be ≤5.7%, confirming that this method was suitable for the "Guidelines for Standard Procedures for Preparing Food Test Methods". The results showed that a total of 151 pesticides (including difenoconazole, deltamethrin, oxyfluorfen, kresoxim-methyl, phosmet, pyrimethanil, tebuconazole, and trifloxystrobin) were detected in 64 of the 100 olive oil products. The detection range of these pesticide residues was 0.01-0.30 mg/kg. The percentage acceptable daily intake (%ADI) of the pesticides calculated using ADI and estimated daily intake (EDI) was 0.0001-0.1346, indicating that the detected pesticides were present at safe levels. This study provides basic data for securing the safety of olive oil products by monitoring pesticide residues in commercially available oilve oil products. Collectively, the analysis method used in this study can be used as a method to analyze residual pesticides in edible oils.
Ryu, Eun Chae;Han, Yun-jeong;Park, Seong-soo;Lim, Chul-joo;Choi, Sunok;Park, Se Chang
Journal of Food Hygiene and Safety
/
v.31
no.2
/
pp.85-93
/
2016
A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.
Due to recent changes in government policy, officetels have received attention as alternative assets, along with the uplift of office and apartment prices in Seoul. However, the current officetel price indexes use small-size samples and, thus, there is a critique on their accuracy. They rely on valuation prices which lag the market trend and do not properly reflect the volatile nature of the property market, resulting in 'smoothing'. Therefore, the purpose of this paper is to create the officetel price index using transaction data. The data, provided by the Ministry of Land, Infrastructure and Transport from 2005 to 2020, includes sales prices and rental prices - Jeonsei and monthly rent (and their combinations). This study employed a repeat sales model for sales, jeonsei, and monthly rent indexes. It also contributes to improving conversion rates (between deposit and monthly rent) as a supplementary indicator. The main findings are as follows. First, the officetel price index and jeonsei index reached 132.5P and 163.9P, respectively, in Q4 2020 (1Q 2011=100.0P). However, the rent index was approximately below 100.0. Sales prices and jeonsei continued to rise due to high demand while monthly rent was largely unchanged due to vacancy risk. Second, the increase in the officetel sales price was lower than other housing types such as apartments and villas. Third, the employed approach has seen a potential to produce more reliable officetel price indexes reflecting high volatility compared to those indexes produced by other institutions, contributing to resolving 'smoothing'. As seen in the application in Seoul, this approach can enhance accuracy and, therefore, better assist market players to understand the market trend, which is much valuable under great uncertainties such as COVID-19 environments.
A simple and sensitive analysis method based on reverse phase (RP) HPCL with flourescence detector was developed for simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE), and their degradation products, $BADGE{\cdot}H_2O$, $BADGE{\cdot}2H_2O$, $BFDGE{\cdot}H_2O$, $BFDGE{\cdot}2H_2O$, $BADGE{\cdot}HCl{\cdot}H_2O$, $BADGE{\cdot}HCl$, $BADGE{\cdot}2HCl$, $BFDGE{\cdot}HCl{\cdot}H_2O$, $BFDGE{\cdot}HCl$ and $BFDGE{\cdot}2HCl$, which were hydrolyzed and chlorinated forms of BADGE and BFDGE, in canned foods and food simulants. These compounds were identified by GC/MSD with $MSTFA-NH_4I-DTE$ derivatization. Recovery study was performed at each 100 ng/mL levels of BPA, BPF, BADGE and BFDGE added to canned foods and food simulants. This method was resulted in recovery of $90{\sim}114%$ with relative standard deviation of $4.1{\sim}7.0%$, detection limits of $6{\sim}11$ ng/mL and quantitation limits of $12{\sim}18\;ng/mL$. Calibration curves were linear with correlatin coefficients of 0.997 for BPF, 0.996 for BPA, 0.9987 for BFDGE, and 0.9989 for BADGE.
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