• Title/Summary/Keyword: calibration

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Validation of an Analytical Method for Deacetylasperulosidic acid, Total Sugar and Monosaccharide Analysis in Fermented Morinda citrifolia Polysaccharide Powder (발효노니 다당체 분말의 deacetylasperulosidic acid, 총당 및 단당류 분석법 검증)

  • Kwon, Heeyeon;Choi, Jisoo;Kim, Soojin;Kim, Eunmin;Uhm, Jihyun;Kim, Bokyung;Lee, Jaeyeon;Kim, Yongdeok
    • Journal of Food Hygiene and Safety
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    • v.37 no.4
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    • pp.216-224
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    • 2022
  • This study was aimed at validating the analysis methods for deacetylasperulosidic acid (DAA), total sugar, galacturonic acid, glucose, and galactose, which are the indicator components of fermented Morinda citrifolia polysaccharide extract (Vitalbos). We modified the previously reported methods for validating the analytical methods. The specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) were measured using phenol-sulfuric acid method and high-performance liquid chromatography (HPLC). The retention time and spectrum of the standard solution of Vitalbos coincided, confirming the specificity. The calibration curve correlation coefficient (R2), of five indicator components, ranged from 0.9995-0.9998, indicating excellent linearity of 0.99 or more. The intra-day and inter-day precision range of the assay was 0.14-3.01%, indicating a precision of less than 5%. The recovery rate was in the range of 95.13-105.59%, presenting excellent accuracy. The LOD ranged from 0.39 to 0.84 ㎍/mL and the LOQ ranged from 1.18 to 2.55 ㎍/mL. Therefore, the analytical method was validated for DAA, total sugar, galacturonic acid, glucose, and galactose, in Vitalbos. The indicator component content in Vitalbos was determined using a validated method. The contents of DAA, total sugar, galacturonic acid, glucose, and galactose were 2.31±0.06, 475.92±5.95, 72.83±1.05, 71.63±2.44, and 67.30±2.31 mg/g of dry weight, respectively. These results suggest that the developed analytical method is efficient and could contribute to the quality control of Vitalbos, as a healthy functional food material.

Characterization of CaCO3 Formation Using an Ion Selective Electrode : Effects of the Mg/Ca Ratio and Temperature (이온 선택성 전극을 이용한 탄산칼슘 형성 특성 연구 : 마그네슘-칼슘 비율과 반응 온도의 영향)

  • Misong Han;Byoung-Young Choi;Seung-Woo, Lee;Jinyoung Park;Soochun Chae;Jun-Hwan Bang;Kyungsun Song
    • Applied Chemistry for Engineering
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    • v.34 no.2
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    • pp.111-120
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    • 2023
  • The nucleation mechanism was studied using a calcium ion selective electrode (Ca ISE) to observe the formation of CaCO3, a representative mineral in the CO2 cycle, and to analyze the effect of the Mg/Ca-ratio and temperature on the formation of pre-nucleation cluster (PNC) and CaCO3. As a result of the experiment, a small amount of crystal was formed. Energy dispersive X-ray spectroscopy (EDS) was used for surface element analysis, and a field emission scanning-electron microscope (FE-SEM) was used for the morphology analysis of synthesized carbonates. These results showed that various shapes of crystalline CaCO3 (calcite, aragonite, etc.) were observed for each Mg/Ca ratio and temperature. In addition, the calibration plot obtained from Ca ISE showed information on the formation process of CaCO3. Our results showed that as magnesium ions interfered with the binding of calcium and carbonate ions and delayed the aggregation between PNCs, the nucleation and formation of CaCO3 were delayed. On the other hand, the temperature showed an opposite trend as compared to the effect of magnesium under our experimental conditions, indicating that temperature accelerated the formation of CaCO3. Furthermore, the morphology of CaCO3 clearly changed according to the Mg/Ca ratio and temperature, and it was confirmed that the two factors are very important for CaCO3 formation in that they could affect the overall process.

Residual evaluation of ethyl formate in soil and crops after fumigation in green house (에틸포메이트의 하우스 농작물 훈증처리 후 토양 및 작물 중 잔류양상)

  • Hwang-Ju Jeon;Kyeongnam Kim;Chaeeun Kim;Yerin Cho;Tae-Hyung Kwon;Byung-Ho Lee;Sung-Eun Lee
    • Korean Journal of Environmental Biology
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    • v.40 no.3
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    • pp.316-324
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    • 2022
  • Ethyl formate (EF) is a potent fumigant replacing methyl bromide. The use of EF is limited to a quarantine process. Appling EF to agricultural field as a safe insecticide in greenhouse give us valuable benefits including less residual concern. In this regard, residual pattern after EF fumigation in greenhouse should be undertaken. In the previous study, we have established agricultural control concentration of EF to control pests in a greenhouse. EF was fumigated at 5 g m-3 level for 2 h. The concentration of EF inside a greenhouse was analyzed to be 4.1-4.3 g m-3 at 30 min after fumigation. To prepare an analytical method for residues in cucumber crops and soil in the greenhouse, the limit of detection(LOD) of the method was 100ng g-1 and the limit of quantitation(LOQ) of this method was 300 ng g-1. R2 values of calibration curves for crops and soil were 0.991-0.997. In samples collected immediately after ventilation, EF concentration was determined to be below LOQ level. In addition, EF level was below LOQ in samples collected at 3 h after ventilation except that leaf samples of melon during the flowering period showed a level of 1,068.9 ng g-1. Taken together, these results indicate that EF used in quarantine can be applied to agricultural fields without residual issue as an effective fumigant for insect pest control.

Square wave voltammetric behaviors and determinations of ranitidine·HCl in the pharmaceutical tablets (의약품 정제 중에 함유된 Ranitidine·HCl의 네모파 전압전류법 거동과 정량분석)

  • Shin, Soon Ho;Hahn, Younghee
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.432-438
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    • 2009
  • In order to develop the analytical method for the pharmaceutical tablets containing ranitidine HCl by square wave voltammetry (SWV), $5.00{\times}10^{-5}M$ ranitidine HCl solutions prepared with phosphate buffers of various pH values were investigated by SWV. The well defined main peak due to the electrochemical reduction of $-NO_2$ in the structure of ranitidine moved towards the cathodic direction by -70 mV/pH as the pH values were increased indicating the involvement of hydrogen in its reduction. The calibration curve, the plot of peak currents (Ip) vs. concentrations of ranitidine HCl in the range between $1.00{\times}10^{-7}M$ and $1.00{\times}10^{-5}M$ showed linearity with slopes of $232,530{\mu}A/M$ (pH 6.14), $289,015{\mu}A/M$ (pH 7.07) and $232,843{\mu}A/M$ (pH 8.01). When one pharmaceutical tablet was simply dissolved in the phosphate buffer with a pH value of 6.14 and determined by standard addition method using SWV, the within-day precision study (n=4) resulted in the contents of ranitidine HCl as $171{\pm}2.1mg$ ($102{\pm}1.3%$ of the specified contents, RSD of 1.2%) in a tablet of Curan$^{(R)}$. The inter-day precision for 5 days was 1.1% of RSD. For Zantac$^{(R)}$ the within-day precision study (n=4) showed the contents of ranitidine HCl as $167{\pm}0.8mg$ ($99{\pm}0.5%$ of the specified contents, RSD of 0.5%) in a tablet and the inter-day precision for 5 days was 0.3% of RSD.

A study of analytical method for Benzo[a]pyrene in edible oils (식용유지 중 벤조피렌 분석법 비교 연구)

  • Min-Jeong Kim;jun-Young Park;Min-Ju Kim;Eun-Young Jo;Mi-Young Park;Nan-Sook Han;Sook-Nam Hwang
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.291-299
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    • 2023
  • The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R2) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

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.

Analysis of the Impact of Satellite Remote Sensing Information on the Prediction Performance of Ungauged Basin Stream Flow Using Data-driven Models (인공위성 원격 탐사 정보가 자료 기반 모형의 미계측 유역 하천유출 예측성능에 미치는 영향 분석)

  • Seo, Jiyu;Jung, Haeun;Won, Jeongeun;Choi, Sijung;Kim, Sangdan
    • Journal of Wetlands Research
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    • v.26 no.2
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    • pp.147-159
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    • 2024
  • Lack of streamflow observations makes model calibration difficult and limits model performance improvement. Satellite-based remote sensing products offer a new alternative as they can be actively utilized to obtain hydrological data. Recently, several studies have shown that artificial intelligence-based solutions are more appropriate than traditional conceptual and physical models. In this study, a data-driven approach combining various recurrent neural networks and decision tree-based algorithms is proposed, and the utilization of satellite remote sensing information for AI training is investigated. The satellite imagery used in this study is from MODIS and SMAP. The proposed approach is validated using publicly available data from 25 watersheds. Inspired by the traditional regionalization approach, a strategy is adopted to learn one data-driven model by integrating data from all basins, and the potential of the proposed approach is evaluated by using a leave-one-out cross-validation regionalization setting to predict streamflow from different basins with one model. The GRU + Light GBM model was found to be a suitable model combination for target basins and showed good streamflow prediction performance in ungauged basins (The average model efficiency coefficient for predicting daily streamflow in 25 ungauged basins is 0.7187) except for the period when streamflow is very small. The influence of satellite remote sensing information was found to be up to 10%, with the additional application of satellite information having a greater impact on streamflow prediction during low or dry seasons than during wet or normal seasons.

Establishment of Analytical Method for Dichlorprop Residues, a Plant Growth Regulator in Agricultural Commodities Using GC/ECD (GC/ECD를 이용한 농산물 중 생장조정제 dichlorprop 잔류 분석법 확립)

  • Lee, Sang-Mok;Kim, Jae-Young;Kim, Tae-Hoon;Lee, Han-Jin;Chang, Moon-Ik;Kim, Hee-Jeong;Cho, Yoon-Jae;Choi, Si-Won;Kim, Myung-Ae;Kim, MeeKyung;Rhee, Gyu-Seek;Lee, Sang-Jae
    • Korean Journal of Environmental Agriculture
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    • v.32 no.3
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    • pp.214-223
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    • 2013
  • BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

The Evaluation of SUV Variations According to the Errors of Entering Parameters in the PET-CT Examinations (PET/CT 검사에서 매개변수 입력오류에 따른 표준섭취계수 평가)

  • Kim, Jia;Hong, Gun Chul;Lee, Hyeok;Choi, Seong Wook
    • The Korean Journal of Nuclear Medicine Technology
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    • v.18 no.1
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    • pp.43-48
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    • 2014
  • Purpose: In the PET/CT images, The SUV (standardized uptake value) enables the quantitative assessment according to the biological changes of organs as the index of distinction whether lesion is malignant or not. Therefore, It is too important to enter parameters correctly that affect to the SUV. The purpose of this study is to evaluate an allowable error range of SUV as measuring the difference of results according to input errors of Activity, Weight, uptake Time among the parameters. Materials and Methods: Three inserts, Hot, Teflon and Air, were situated in the 1994 NEMA Phantom. Phantom was filled with 27.3 MBq/mL of 18F-FDG. The ratio of hotspot area activity to background area activity was regulated as 4:1. After scanning, Image was re-reconstructed after incurring input errors in Activity, Weight, uptake Time parameters as ${\pm}5%$, 10%, 15%, 30%, 50% from original data. ROIs (region of interests) were set one in the each insert areas and four in the background areas. $SUV_{mean}$ and percentage differences were calculated and compared in each areas. Results: $SUV_{mean}$ of Hot. Teflon, Air and BKG (Background) areas of original images were 4.5, 0.02. 0.1 and 1.0. The min and max value of $SUV_{mean}$ according to change of Activity error were 3.0 and 9.0 in Hot, 0.01 and 0.04 in Teflon, 0.1 and 0.3 in Air, 0.6 and 2.0 in BKG areas. And percentage differences were equally from -33% to 100%. In case of Weight error showed $SUV_{mean}$ as 2.2 and 6.7 in Hot, 0.01 and 0.03 in Tefron, 0.09 and 0.28 in Air, 0.5 and 1.5 in BKG areas. And percentage differences were equally from -50% to 50% except Teflon area's percentage deference that was from -50% to 52%. In case of uptake Time error showed $SUV_{mean}$ as 3.8 and 5.3 in Hot, 0.01 and 0.02 in Teflon, 0.1 and 0.2 in Air, 0.8 and 1.2 in BKG areas. And percentage differences were equally from 17% to -14% in Hot and BKG areas. Teflon area's percentage difference was from -50% to 52% and Air area's one was from -12% to 20%. Conclusion: As shown in the results, It was applied within ${\pm}5%$ of Activity and Weight errors if the allowable error range was configured within 5%. So, The calibration of dose calibrator and weighing machine has to conduct within ${\pm}5%$ error range because they can affect to Activity and Weight rates. In case of Time error, it showed separate error ranges according to the type of inserts. It showed within 5% error when Hot and BKG areas error were within ${\pm}15%$. So we have to consider each time errors if we use more than two clocks included scanner's one during the examinations.

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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.