• Title/Summary/Keyword: Phase variation

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Analytical Method for Sodium Polyacrylate in Processed Food Products by Using Size-exclusion Chromatography (Size-exclusion Chromatography를 활용한 가공식품 중 폴리아크릴산나트륨 분석법 확립)

  • Jeong, Eun-Jeong;Choi, Yoo-Jeong;Lee, Gunyoung;Yun, Sang Soon;Lim, Ho Soo;Kim, MeeKyung;Kim, Yong-Suk
    • Journal of Food Hygiene and Safety
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    • v.33 no.6
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    • pp.466-473
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    • 2018
  • An analytical method of sodium polyacrylate in processed food products was developed and monitored by using size-exclusion chromatography. GF-7M HQ column and UV/VIS detector were selected based on peak shape and linearity. Flow rate, column oven temperature, and mobile phase were selected as 0.6 mL/min, $45^{\circ}C$, and 50 mM sodium phosphate buffer of pH 9.0, respectively. Samples for analysis of sodium polyacrylate were extracted with 50 mM sodium phosphate buffer of pH 7.0 for 3 hr at $20^{\circ}C$ and 150 rpm. Analytical method validation revealed proper selectivity and calibration curve was selected in the range of 50-500 mg/L, and correlation coefficient of calibration curve was more than 0.9985. Limit of detection of sodium polyacrylate was 10.95 mg/kg and limit of quantification was 33.19 mg/kg. Accuracy and coefficient of variation for sodium polyacrylate analysis was 99.6-127.6%, 3.0-8.3% for intra-day and 94.3-121.9%, 1.3-2.6% for inter-day, respectively. Sodium polyacrylate was detected in 40 samples among monitored 125 processed food products. Detected contents were less than 0.2%, limited by the Food Additives Code. Results suggest the established size-exclusion chromatography method could be used to analyze sodium polyacrylate in processed food products.

Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

Performance Prediction for an Adaptive Optics System Using Two Analysis Methods: Statistical Analysis and Computational Simulation (통계분석 및 전산모사 기법을 이용한 적응광학 시스템 성능 예측)

  • Han, Seok Gi;Joo, Ji Yong;Lee, Jun Ho;Park, Sang Yeong;Kim, Young Soo;Jung, Yong Suk;Jung, Do Hwan;Huh, Joon;Lee, Kihun
    • Korean Journal of Optics and Photonics
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    • v.33 no.4
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    • pp.167-176
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    • 2022
  • Adaptive optics (AO) systems compensate for atmospheric disturbance, especially phase distortion, by introducing counter-wavefront deformation calculated from real-time wavefront sensing or prediction. Because AO system implementations are time-consuming and costly, it is highly desirable to estimate the system's performance during the development of the AO system or its parts. Among several techniques, we mostly apply statistical analysis, computational simulation, and optical-bench tests. Statistical analysis estimates performance based on the sum of performance variances due to all design parameters, but ignores any correlation between them. Computational simulation models every part of an adaptive optics system, including atmospheric disturbance and a closed loop between wavefront sensor and deformable mirror, as close as possible to reality, but there are still some differences between simulation models and reality. The optical-bench test implements an almost identical AO system on an optical bench, to confirm the predictions of the previous methods. We are currently developing an AO system for a 1.6-m ground telescope using a deformable mirror that was recently developed in South Korea. This paper reports the results of the statistical analysis and computer simulation for the system's design and confirmation. For the analysis, we apply the Strehl ratio as the performance criterion, and the median seeing conditions at the Bohyun observatory in Korea. The statistical analysis predicts a Strehl ratio of 0.31. The simulation method similarly reports a slightly larger value of 0.32. During the study, the simulation method exhibits run-to-run variation due to the random nature of atmospheric disturbance, which converges when the simulation time is longer than 0.9 seconds, i.e., approximately 240 times the critical time constant of the applied atmospheric disturbance.

Influence of Increased Carbon Dioxide Concentration on the Bioluminescence and Cell Density of Marine Bacteria Vibrio fischeri (이산화탄소 농도 증가에 따른 발광미생물의 상대발광량과 밀도변화에 대한 연구)

  • Sung, Chan-Gyoung;Moom, Seong-Dae;Kim, Hye-Jin;Choi, Tae-Seob;Lee, Kyu-Tae;Lee, Jung-Suk;Kang, Seong-Gil
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.15 no.1
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    • pp.8-15
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    • 2010
  • An experiment was conducted to evaluate the biologically adverse effect of increased carbon dioxide in seawater on marine bacteria, Vibrio fischeri. We measured the bioluminescence and cell density at every 6 hours for 24 hours of the whole incubation period after exposing test microbes to a range of $CO_2$ concentration such as 380(Control), 1,000, 3,000, 10,000 and 30,000 ppm, respectively. Significant effect on relative luminescence(RLU) of V. fischeri was observed in treatments with $CO_2$ concentration higher than 3,000 ppm at t=12 h. However, the difference of RLU among treatments significantly decreased with the incubation time until t=24 h. Similar trend was observed for the variation of cell density, which was measured as optical density using spectrophotometer. The results showed that a significant relationship between $CO_2$ concentration and bioluminescence of test microbes was observed for the mean time. However, the inhibition of relative bioluminescence and also cell density could be recovered at the concentration levels higher than 3,000 ppm. The dissolved $CO_2$ can be absorbed directly by cell and it can decrease the intracellular pH. Our results implied that microbes might be adversely affected at the initial growing phase by increased $CO_2$. However, they could adapt by increasing ion transport including bicarbonate and then could make their pH back to normal level. Results of this study could be supported to understand the possible influence on marine bacteria by atmospheric increase of $CO_2$ in near future and also by released $CO_2$ during the marine $CO_2$ sequestration activity.

Mineral Nutrition of the Field-Grown Rice Plant -[I] Recovery of Fertilizer Nitrogen, Phosphorus and Potassium in Relation to Nutrient Uptake, Grain and Dry Matter Yield- (포장재배(圃場栽培) 수도(水稻)의 무기영양(無機營養) -[I] 삼요소이용률(三要素利用率)과 양분흡수량(養分吸收量), 수량(收量) 및 건물생산량(乾物生産量)과(乾物生産量)의 관계(關係)-)

  • Park, Hoon
    • Applied Biological Chemistry
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    • v.16 no.2
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    • pp.99-111
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    • 1973
  • Percentage recovery or fertilizer nitrogen, phosphorus and potassium by rice plant(Oriza sativa L.) were investigated at 8, 10, 12, 14 kg/10a of N, 6 kg of $P_2O_5$ and 8 kg of $K_2O$ application level in 1967 (51 places) and 1968 (32 places). Two types of nutrient contribution for the yield, that is, P type in which phosphorus firstly increases silicate uptake and secondly silicate increases nitrogen uptake, and K type in which potassium firstly increases P uptake and secondly P increases nitrogen uptake were postulated according to the following results from the correlation analyses (linear) between percentage recovery of fertilizer nutrient and grain or dry matter yields and nutrient uptake. 1. Percentage frequency of minus or zero recovery occurrence was 4% in nitrogen, 48% in phosphorus and 38% in potassium. The frequency distribution of percentage recovery appeared as a normal distribution curve with maximum at 30 to 40 recovery class in nitrogen, but appeared as a show distribution with maximum at below zero class in phosphorus and potassium. 2. Percentage recovery (including only above zero) was 33 in N (above 10kg/10a), 27 in P, 40 in K in 1967 and 40 in N, 20 in P, 46 in Kin 1968. Mean percentage recovery of two years including zero for zero or below zero was 33 in N, 13 in P and 27 in K. 3. Standard deviation of percentage recovery was greater than percentage recovery in P and K and annual variation of CV (coefficient of variation) was greatest in P. 4. The frequency of significant correlation between percentage recovery and grain or dry matter yield was highest in N and lowest in P. Percentage recovery of nitrogen at 10 kg level has significant correlation only with percentage recovery of P in 1967 and only with that of potassium in 1968. 5. The correlation between percentage recovery and dry matter yield of all treatments showed only significant in P in 1967, and only significant in K in 1968, Negative correlation coefficients between percentage recovery and grain or dry matter yield of no or minus fertilizer plots were shown only in K in 1967 and only in P in 1968 indicating that phosphorus fertilizer gave a distinct positive role in 1967 but somewhat' negative role in 1968 while potassium fertilizer worked positively in 1968 but somewhat negatively in 1967. 6. The correlation between percentage recovery of nutrient and grain yield showed similar tendency as with dry matter yield but lower coefficients. Thus the role of nutrients was more precisely expressed through dry matter yield. 7. Percentage recovery of N very frequently had significant correlation with nitrogen uptake of nitrogen applied plot, and significant negative correlation with nitrogen uptake of minus nitrogen plot, and less frequently had significant correlation with P, K and Si uptake of nitrogen applied plot. 8. Percentage recovery of P had significant correlation with Si uptake of all treatments and with N uptake of all treatments except minus phosphorus plot in 1967 indicating that phosphorus application firstly increases Si uptake and secondly silicate increases nitrogen uptake. Percentage recovery of P also frequently had significant correlation with P or K uptake of nitrogen applied plot. 9. Percentage recovery of K had significant correlation with P uptake of all treatments, N uptake of all treatments except minus phosphorus plot, and significant negative correlation with K uptake of minus K plot and with Si uptake of no fertilizer plot or the highest N applied plot in 1968, and negative correlation coefficient with P uptake of no fertilizer or minus nutrient plot in 1967. Percentage recovery of K had higher correlation coefficients with dry matter yield or grain yield than with K uptake. The above facts suggest that K application firstly increases P uptake and secondly phosphorus increases nitrogen uptake for dry matter yied. 10. Percentage recovery of N had significant higher correlation coefficient with grain yield or dry matter yield of minus K plot than with those of minus phosphorus plot, and had higher with those of fertilizer plot than with those of minus K plot. Similar tendency was observed between N uptake and percentage recovery of N among the above treatments. Percentage recovery of K had negative correlation coefficient with grain or-dry matter yield of no fertilizer plot or minus nutrient plot. These facts reveal that phosphorus increases nitrogen uptake and when phosphorus or nitrogen is insufficient potassium competatively inhibits nitrogen uptake. 11. Percentage recovery of N, Pand K had significant negative correlation with relative dry matter yield of minus phosphorus plot (yield of minus plot x 100/yield of complete plot; in 1967 and with relative grain yield of minus K plot in 1968. These results suggest that phosphorus affects tillering or vegetative phase more while potassium affects grain formation or Reproductive phase more, and that clearly show the annual difference of P and K fertilizer effect according to the weather. 12. The correlation between percentage recovery of fertilizer and the relative yield of minus nutrient plat or that of no fertilizer plot to that of minus nutrient plot indicated that nitrogen is the most effective factor for the production even in the minus P or K plot. 13. From the above facts it could be concluded that about 40 to 50 percen of paddy fields do rot require P or K fertilizer and even in the case of need the application amount should be greatly different according to field and weather of the year, especially in phosphorus.

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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.

Time Course Variation of Vitamin $C_3$ Content in Leg Skin of Broiler Chicks Exposed to Different Dose of UVB Light (자외선의 상이한 선양을 조사한 브로일러 병아리의 다리 피부중 비타민 $C_3$ 함양의 경시적 변화)

  • 장윤환;김강수;여영수;강훈석;조인호;배은경
    • Korean Journal of Poultry Science
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    • v.20 no.2
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    • pp.93-105
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    • 1993
  • This study was carried out to determine the concentrations of previtamin D$_3$(PreD$_3$), lumisterol$_3$(L3), tachystero1$_3$(73), vitamin D$_3$(VD$_3$) and provitamin D$_3$(ProD$_3$) in leg skins of broiler chicks exposed to UVB lights (maximum intensity at 297 nm) with dose of 0.204 or 0.409 mJ/$\textrm{cm}^2$(30 or 60 min irradiation) . The broiler Hubbard line day old chicks(2 dose $\times$9 elapsed time $\times$4 replica+10 control=82) were fed VD-deficient diet for 31 days in a windowless subdued light room. The skin was collected at 0, 6, 12, 18, 30, 42, 66, 90 or 138 hr after UVB irradiation. The skin lipid was extracted by 9% ethyl acetate/n-hexane, and the fraction of VD$_3$ and its analogues was purified by Sep-Pak silica cartridge. The straight phase HPLC was utilized to analyze ProD$_3$ and its products. The mole %(absolute level expressed in ng/$\textrm{cm}^2$) of PreD$_3$ in leg skin (epidermis+dermis) was 4.67%(44 ng/$\textrm{cm}^2$) or 3.97%(37 ng/$\textrm{cm}^2$) right after UVB irradiation by 0.204 or 0.409 mJ/$\textrm{cm}^2$(30 or 60 min) at 15 cm distance, respectively. It content in leg skin at 0 hr after exposure was 7.24%(12 ng/$\textrm{cm}^2$) or 0.92%(9 ng/$\textrm{cm}^2$), respectively. The increase in irradiation dose did not affect proportionally the If synthesis.73 concentration in leg skin was 0.58%(S ng/$\textrm{cm}^2$) or 0.57%(6 ng/$\textrm{cm}^2$), respectively 0 hr after irradiation. The VD$_3$ in leg skin of birds exposed to UVB light with dose of 0.204 or 0.409 mJ/$\textrm{cm}^2$ was 2.13% (21 ng/$\textrm{cm}^2$) or 0.97% (16ng/$\textrm{cm}^2$), respectively at 0 hr after exposure, 2.72%(26ng/$\textrm{cm}^2$) or 3.84%(37ng/$\textrm{cm}^2$), respectively at 6 hr, and 4.30% ((33ng/$\textrm{cm}^2$) or 6.40%(76ng/$\textrm{cm}^2$), respectively at 12 hr. The peak concentration of VD$_3$ was presented at 18 or 30 hr when 0.204 or 0.409 mJ/$\textrm{cm}^2$) was treated, respectively. It was shown that 18~30 hr were necessary for the thermal conversion of PreD$_3$ into VD$_3$ in the leg skin of broiler chicks. The ProD$_3$ contents in leg skins of negative control, 0.204 mJ/$\textrm{cm}^2$ and 0.409 mJ/$\textrm{cm}^2$ treated birds were 966, 948 and 815 ng/$\textrm{cm}^2$, respectively at right before and after UVB exposure. It was estimated that 18 or 151 ng/$\textrm{cm}^2$ of ProD$_3$ was isomerized to PreD$_3$, L$_3$, T$_3$ and VD$_3$ when exposed to 0.204 or 0.409 mJ/$\textrm{cm}^2$, respective)y. Consequently it was shown that when double dose of UVB light was applied to irradiate the chick body, more but not double synthesis of VD$_3$ and its analogues was occured in leg skin of brolier chicks.

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