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Improvement of an Analytical Method for Methoprene in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 살충제 메토프렌의 잔류분석법 개선)

  • Park, Eun-Ji;Kim, Nam Young;Park, So-Ra;Lee, Jung Mi;Jung, Yong Hyun;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.37 no.3
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    • pp.136-142
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    • 2022
  • The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO4, primary secondary amine (PSA), and octadecyl (C18), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R2) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

Report about First Repeated Sectional Measurements of Water Property in the East Sea using Underwater Glider (수중글라이더를 활용한 동해 최초 연속 물성 단면 관측 보고)

  • GYUCHANG LIM;JONGJIN PARK
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.29 no.1
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    • pp.56-76
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    • 2024
  • We for the first time made a successful longest continuous sectional observation in the East Sea by an underwater glider during 95 days from September 18 to December 21 2020 in the Korea along the 106 Line (129.1 °E ~ 131.5 °E at 37.9 °N) of the regular shipboard measurements by the National Institute of Fishery Science (NIFS) and obtained twelve hydrographic sections with high spatiotemporal resolution. The glider was deployed at 129.1 °E in September 18 and conducted 88-days flight from September 19 to December 15 2020, yielding twelve hydrographic sections, and then recovered at 129.2 °E in December 21 after the last 6 days virtual mooring operation. During the total traveled distance of 2550 km, the estimated deviation from the predetermined zonal path had an average RMS distance of 262 m. Based on these high-resolution long-term glider measurements, we conducted a comparative study with the bi-monthly NIFS measurements in terms of spatial and temporal resolutions, and found distinguished features. One is that spatial features of sub-mesoscale such as sub-mesoscale frontal structure and intensified thermocline were detected only in the glider measurements, mainly due to glider's high spatial resolution. The other is the detection of intramonthly variations from the weekly time series of temperature and salinity, which were extracted from glider's continuous sections. Lastly, there were deviations and bias in measurements from both platforms. We argued these deviations in terms of the time scale of variation, the spatial scale of fixed-point observation, and the calibration status of CTD devices of both platforms.

Improvement and Validation of an Analytical Method for Quercetin-3-𝑜-gentiobioside and Isoquercitrin in Abelmoschus esculentus L. Moench (오크라 분말의 Quercetin-3-𝑜-Gentiobioside 및 Isoquercitrin의 분석법 개선 및 검증)

  • Han, Xionggao;Choi, Sun-Il;Men, Xiao;Lee, Se-jeong;Jin, Heegu;Oh, Hyun-Ji;Cho, Sehaeng;Lee, Boo-Yong;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.37 no.2
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    • pp.39-45
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    • 2022
  • This study aimed to investigate the validation and modify the analytical method to determine quercetin-3-𝑜-gentiobioside and isoquercitrin in Abelmoschus esculentus L. Moench for the standardization of ingredients in development of functional health products. The analytical method was validated based on the ICH (International Conference for Harmonization) guidelines to verify the reliability and validity there of on the specificity, linearity, accuracy, precision, detection limit and quantification limit. For the HPLC analysis method, the peak retention time of the index component of the standard solution and the peak retention time of the index component of A. esculentus L. Moench powder sample were consistent with the spectra thereof, confirming the specificity. The calibration curves of quercetin-3-𝑜-gentiobioside and isoquercitrin showed a linearity with a near-one correlation coefficient (0.9999 and 0.9999), indicating the high suitability thereof for the analysis. A. esculentus L. Moench powder sample of a known concentration were prepared with low, medium, and high concentrations of standard substances and were calculated for the precision and accuracy. The precision of quercetin-3-𝑜-gentiobioside and isoquercitrin was confirmed for intra-day and daily. As a result, the intra-day precision was found to be 0.50-1.48% and 0.77-2.87%, and the daily precision to be 0.07-3.37% and 0.58-1.37%, implying an excellent precision at level below 5%. As a result of accuracy measurement, the intra-day accuracy of quercetin-3-𝑜-gentiobioside and isoquercitrin was found to be 104.87-109.64% and the daily accuracy thereof was found to be 106.85-109.06%, reflecting high level of accuracy. The detection limits of quercetin-3-𝑜-gentiobioside and isoquercitrin were 0.24 ㎍/mL and 0.16 ㎍/mL, respectively, whereas the quantitation limits were 0.71 ㎍/mL and 0.49 ㎍/mL, confirming that detection was valid at the low concentrations as well. From the analysis, the established analytical method was proven to be excellent with high level of results from the verification on the specificity, linearity, precision, accuracy, detection limit and quantitation limit thereof. In addition, as a result of analyzing the content of A. esculentus L. Moench powder samples using a validated analytical method, quercetin-3-𝑜-gentiobioside was analyzed to contain 1.49±0.01 mg/dry weight g, while isoquercitrin contained 1.39±0.01 mg/dry weight g. The study was conducted to verify that the simultaneous analysis on quercetin-3-𝑜-gentiobioside and isoquercitrin, the indicators of A. esculentus L. Moench, is a scientifically reliable and suitable analytical method.

Estimation of Fresh Weight and Leaf Area Index of Soybean (Glycine max) Using Multi-year Spectral Data (다년도 분광 데이터를 이용한 콩의 생체중, 엽면적 지수 추정)

  • Jang, Si-Hyeong;Ryu, Chan-Seok;Kang, Ye-Seong;Park, Jun-Woo;Kim, Tae-Yang;Kang, Kyung-Suk;Park, Min-Jun;Baek, Hyun-Chan;Park, Yu-hyeon;Kang, Dong-woo;Zou, Kunyan;Kim, Min-Cheol;Kwon, Yeon-Ju;Han, Seung-ah;Jun, Tae-Hwan
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.23 no.4
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    • pp.329-339
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    • 2021
  • Soybeans (Glycine max), one of major upland crops, require precise management of environmental conditions, such as temperature, water, and soil, during cultivation since they are sensitive to environmental changes. Application of spectral technologies that measure the physiological state of crops remotely has great potential for improving quality and productivity of the soybean by estimating yields, physiological stresses, and diseases. In this study, we developed and validated a soybean growth prediction model using multispectral imagery. We conducted a linear regression analysis between vegetation indices and soybean growth data (fresh weight and LAI) obtained at Miryang fields. The linear regression model was validated at Goesan fields. It was found that the model based on green ratio vegetation index (GRVI) had the greatest performance in prediction of fresh weight at the calibration stage (R2=0.74, RMSE=246 g/m2, RE=34.2%). In the validation stage, RMSE and RE of the model were 392 g/m2 and 32%, respectively. The errors of the model differed by cropping system, For example, RMSE and RE of model in single crop fields were 315 g/m2 and 26%, respectively. On the other hand, the model had greater values of RMSE (381 g/m2) and RE (31%) in double crop fields. As a result of developing models for predicting a fresh weight into two years (2018+2020) with similar accumulated temperature (AT) in three years and a single year (2019) that was different from that AT, the prediction performance of a single year model was better than a two years model. Consequently, compared with those models divided by AT and a three years model, RMSE of a single crop fields were improved by about 29.1%. However, those of double crop fields decreased by about 19.6%. When environmental factors are used along with, spectral data, the reliability of soybean growth prediction can be achieved various environmental conditions.

Simultaneous Determination of Fructose, Glucose, and Sucrose in Honey and Commercial Drinks by GC and GC/MS (GC 및 GC/MS를 이용한 벌꿀 및 시판 음료 중의 Fructose, Glucose 및 Sucrose의 동시분석)

  • Yun, Jeong-Sik;Jeon, Hyun-Suk;Kim, In-Suk;Lee, Hee-Jin;Lee, Hye-Jeong;Hyun, Jae-Yeoul;Kim, Jong-Bae
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.537-544
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    • 2013
  • This study was performed to establish method of simultaneous determination of fructose, glucose, and sucrose in honey and commercial vitamin drinks by GC and GC/MS. Optimum chromatographic separation of trimethylsilyl-oxime (TMSO) derivatives by GC was achieved on a DB-5 column. Calibration curves for fructose, glucose and sucrose TMSO derivatives by GC were linear in the range of 50-5000 ${\mu}g/mL$, and their $r^2$ values were 0.9999, The limit of detection and limit of quantification of fructose, glucose, and sucrose were 0.68, 0.47, and 0.53 ${\mu}g/mL$, respectively, and 2.27, 1.58, and 1.77 ${\mu}g/mL$, respectively. Average recoveries of fructose, glucose, and sucrose were 100.5, 101.0, and 99.7%, respectively. When the method was applied to 12 honey samples, the average concentrations of fructose, glucose and sucrose were $42.58{\pm}1.97%$, $27.74{\pm}1.16%$, and $0.79{\pm}0.52%$, respectively. The F/G ratio was $1.53{\pm}0.07$. For fructose and glucose contents, results from the GC analysis were similar to those from the HPLC analysis, but the sucrose content was different for each analysis method. We suggest that the GC method is more suitable than other official analytical methods for simultaneous determination of fructose, glucose, and sucrose in honey.

Multi-residue Pesticide Analysis in Cereal using Modified QuEChERS Samloe Preparation Method (곡물류 중 잔류농약 다성분 분석을 위한 개선된 QuEChERS 시료 정제법의 개발)

  • Yang, In-Cheol;Hong, Su-Myeong;Kwon, Hye-Young;Kim, Taek-Kyum;Kim, Doo-Ho
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.314-334
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    • 2013
  • This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

Development and Validation of Analytical Method for Nitroxoline in Chicken Using HPLC-PDA (HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Eun;Kim, Jae-Young;Kang, Ilhyun;Lee, Sang-Mok;Do, Jung-Ah;Oh, Jae-Ho;Chang, Moon-Ik;Hong, Jin-Hwan
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.70-77
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    • 2013
  • BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

Assessment of future climate and land use changes impact on hydrologic behavior in Anseong-cheon Gongdo urban-growing watershed (미래 기후변화와 토지이용변화가 안성천 공도 도시성장 유역의 수문에 미치는 영향 평가)

  • Kim, Da Rae;Lee, Yong Gwan;Lee, Ji Wan;Kim, Seong Joon
    • Journal of Korea Water Resources Association
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    • v.51 no.2
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    • pp.141-150
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    • 2018
  • The purpose of this study is to evaluate the future hydrologic behavior affected by the potential climate and land use changes in upstream of Anseong-cheon watershed ($366.5km^2$) using SWAT. The HadGEM3-RA RCP 4.5 and 8.5 scenarios were used for 2030s (2020-2039) and 2050s (2040-2059) periods as the future climate change scenario. It was shown that maximum changes of precipitation ranged from -5.7% in 2030s to +18.5% in 2050s for RCP 4.5 scenarios and the temperature increased up to $1.8^{\circ}C$ and $2.6^{\circ}C$ in 2030s RCP 4.5 and 2050s 8.5 scenarios respectively based on baseline (1976-2005) period. The future land uses were predicted using the CLUE-s model by establishing logistic regression equation. The 2050 urban area were predicted to increase of 58.6% (29.0 to $46.0km^2$). The SWAT was calibrated and verified using 14 years (2002-2015) of daily streamflow with 0.86 and 0.76 Nash-Sutcliffe model efficiency (NSE) for stream flow (Q) and low flow 1/Q respectively focusing on 2 drought years (2014-2015) calibration. For future climate change only, the stream discharge showed maximum decrease of 24.2% in 2030s RCP 4.5 and turned to maximum increase of 10.9% in 2050s RCP 4.5 scenario compared with the baseline period stream discharge of 601.0 mm by the precipitation variation and gradual temperature increase. While considering both future climate and land use change, the stream discharge showed maximum decrease of 14.9% in 2030s RCP 4.5 and maximum increase of 19.5% in 2050s RCP 4.5 scenario by the urban growth and the related land use changes. The results supported that the future land use factor might be considered especially for having high potential urban growth within a watershed in the future climate change assessment.

Determination of finasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 finasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.345-351
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    • 2011
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

Determination of secondary aliphatic amines in surface and tap waters as benzenesulfonamide derivatives using GC-MS (Benzenesulfonamide 유도체로 GC-MS를 사용한 지표수 및 수돗물 중 2차 지방족 아민의 분석)

  • Park, Sunyoung;Jung, Sungjin;Kim, Yunjeong;Kim, Hekap
    • Analytical Science and Technology
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    • v.31 no.2
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    • pp.96-105
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    • 2018
  • This study aimed to improve the method for detecting eight secondary aliphatic amines (SAAs), so as to measure their concentrations in fresh water and tap water samples. NaOH (8 mL, 10 M) and benzenesulfonyl chloride (2 mL) were added to a water sample (200 mL), and the mixture was stirred at $80^{\circ}C$ for 30 min. An additional NaOH solution (10 mL) was added and the stirring was continued for another 30 min. The pH of the cooled mixture was adjusted to 5.5-6.0 by adding HCl (35 %), and the SAAs were extracted using dichloromethane (50 mL). This extraction was repeated once. The extract was then washed with $NaHCO_3$ (15 mL, 0.05 M) and dried over $Na_2SO_4$ (4 g). The extract was finally concentrated to 0.1 mL, of which $1{\mu}L$ was analyzed for SAAs by GC-MS. The linearity of the spike calibration curves was high ($r^2=0.9969-0.9996$). The detection limits of the method ranged from 0.01 to $0.20{\mu}g/L$, and its repeatability and reproducibility (expressed as relative standard deviation) were both less than 10 % (6.6-9.4 %). Its accuracy (measured in percentage error) ranged between 2.4 % and 6.1 %. The established method was applied to the analysis of five surface water and 82 tap water samples. Dimethylamine was the only SAA detected in all the water samples, and its average concentration was $0.79{\mu}g/L$ (range: $0.20-2.54{\mu}g/L$). Therefore, this study improved the analytical method for SAAs in surface water and tap water, and the regional and seasonal concentration distributions were obtained.