• Title/Summary/Keyword: Validation Study

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Development and Validation of an Analytical Method for the Insecticide Sulfoxaflor in Agricultural Commodities using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 살충제 sulfoxaflor의 시험법 개발 및 검증)

  • Do, Jung-Ah;Lee, Mi-Young;Park, Hyejin;Kwon, Ji-Eun;Jang, Hyojin;Cho, Yoon-Jae;Kang, Il-Hyun;Lee, Sang-Mok;Chang, Moon-Ik;Oh, Jae-Ho;Hwang, In-Gyun
    • Korean Journal of Food Science and Technology
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    • v.45 no.2
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    • pp.148-155
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    • 2013
  • 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.

Intra-laboratory Validation of an HPLC Post-column Oxidation Method for the Analysis of PSP Toxins in Oysters and Mussels (굴과 진주담치 중 마비성 패류독소 분석을 위한 HPLC post-column oxidation method의 시험소 내 유효성 검증)

  • Song, Ki Cheol;Lee, Ka-Jeong;Yu, Hong-Sik;Mok, Jong-Soo;Kim, Ji Hoe;Lim, Keun-Sik;Lee, Mi-Ae;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.45 no.2
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    • pp.241-247
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    • 2013
  • AOAC Mouse Bioassay Analysis (MBA) has been the gold standard for the analysis of paralytic shellfish poisoning toxin (PSP toxin) for more than 50 years. However, this method has inaccurate limit of quantification and cannot be used to determine toxic profiles. An HPLC method (PCOX) was optimized for Korean shellfish to establish an alternative or supplementary method for PSP analysis and was intended to be used for the official monitoring and regulation of food. The recovery rate of the PCOX method was 83.5-112.1% and the limit of quantification for total toxin was about $8.6{\mu}g$/100 g. A long-term comparison study showed a good correlation of the PCOX results with the AOAC MBA results: the correlation factors were 0.9534 and 0.9109 for oyster and mussel matrices, respectively. The PCOX method may be used as an alternative or supplementary method for AOAC MBA to monitor the occurrence of PSP and to analyze PSP toxin profile in oysters and mussels.

Operational Ship Monitoring Based on Multi-platforms (Satellite, UAV, HF Radar, AIS) (다중 플랫폼(위성, 무인기, AIS, HF 레이더)에 기반한 시나리오별 선박탐지 모니터링)

  • Kim, Sang-Wan;Kim, Donghan;Lee, Yoon-Kyung;Lee, Impyeong;Lee, Sangho;Kim, Junghoon;Kim, Keunyong;Ryu, Joo-Hyung
    • Korean Journal of Remote Sensing
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    • v.36 no.2_2
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    • pp.379-399
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    • 2020
  • The detection of illegal ship is one of the key factors in building a marine surveillance system. Effective marine surveillance requires the means for continuous monitoring over a wide area. In this study, the possibility of ship detection monitoring based on satellite SAR, HF radar, UAV and AIS integration was investigated. Considering the characteristics of time and spatial resolution for each platform, the ship monitoring scenario consisted of a regular surveillance system using HFR data and AIS data, and an event monitoring system using satellites and UAVs. The regular surveillance system still has limitations in detecting a small ship and accuracy due to the low spatial resolution of HF radar data. However, the event monitoring system using satellite SAR data effectively detects illegal ships using AIS data, and the ship speed and heading direction estimated from SAR images or ship tracking information using HF radar data can be used as the main information for the transition to UAV monitoring. For the validation of monitoring scenario, a comprehensive field experiment was conducted from June 25 to June 26, 2019, at the west side of Hongwon Port in Seocheon. KOMPSAT-5 SAR images, UAV data, HF radar data and AIS data were successfully collected and analyzed by applying each developed algorithm. The developed system will be the basis for the regular and event ship monitoring scenarios as well as the visualization of data and analysis results collected from multiple platforms.

Neutrophil Count and the Inflammation-based Glasgow Prognostic Score Predict Survival in Patients with Advanced Gastric Cancer Receiving First-line Chemotherapy

  • Li, Qing-Qing;Lu, Zhi-Hao;Yang, Li;Lu, Ming;Zhang, Xiao-Tian;Li, Jian;Zhou, Jun;Wang, Xi-Cheng;Gong, Ji-Fang;Gao, Jing;Li, Jie;Li, Yan;Shen, Lin
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.2
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    • pp.945-950
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    • 2014
  • Purpose: To explore the value of systemic inflammatory markers as independent prognostic factors and the extent these markers improve prognostic classification for patients with inoperable advanced or metastatic gastric cancer (GC) receiving palliative chemotherapy. Methods: We studied the prognostic value of systemic inflammatory factors such as circulating white blood cell count and its components as well as that combined to form inflammation-based prognostic scores (Glasgow Prognostic Score (GPS), Neutrophil-Lymphocyte Ratio (NLR), Platelet Lymphocyte Ratio (PLR), Prognostic Index (PI) and Prognostic Nutritional Index (PNI)) in 384 patients with inoperable advanced or metastatic gastric cancer (GC) receiving first-line chemotherapy. Univariate and multivariate analyses were performed to examine the impact of inflammatory markers on overall survival (OS). Results: Univariate analysis revealed that an elevated white blood cell, neutrophil and/or platelet count, a decreased lymphocyte count, a low serum albumin concentration, and high CRP concentration, as well as elevated NLR/PLR, GPS, PI, PNI were significant predictors of shorter OS. Multivariate analysis demonstrated that only elevated neutrophil count (HR 3.696, p=0.003) and higher GPS (HR 1.621, p=0.01) were independent predictors of poor OS. Conclusion: This study demonstrated elevated pretreatment neutrophil count and high GPS to be independent predictors of shorter OS in inoperable advanced or metastatic GC patients treated with first-line chemotherapy. Upon validation of these data in independent studies, stratification of patients using these markers in future clinical trials is recommended.

Design and Optimization of Pilot-Scale Bunsen Process in Sulfur-Iodine (SI) Cycle for Hydrogen Production (수소 생산을 위한 Sulfur-Iodine Cycle 분젠반응의 Pilot-Scale 공정 모델 개발 및 공정 최적화)

  • Park, Junkyu;Nam, KiJeon;Heo, SungKu;Lee, Jonggyu;Lee, In-Beum;Yoo, ChangKyoo
    • Korean Chemical Engineering Research
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    • v.58 no.2
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    • pp.235-247
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    • 2020
  • Simulation study and validation on 50 L/hr pilot-scale Bunsen process was carried out in order to investigate thermodynamics parameters, suitable reactor type, separator configuration, and the optimal conditions of reactors and separation. Sulfur-Iodine is thermochemical process using iodine and sulfur compounds for producing hydrogen from decomposition of water as net reaction. Understanding in phase separation and reaction of Bunsen Process is crucial since Bunsen Process acts as an intermediate process among three reactions. Electrolyte Non-Random Two-Liquid model is implemented in simulation as thermodynamic model. The simulation results are validated with the thermodynamic parameters and the 50 L/hr pilot-scale experimental data. The SO2 conversions of PFR and CSTR were compared as varying the temperature and reactor volume in order to investigate suitable type of reactor. Impurities in H2SO4 phase and HIX phase were investigated for 3-phase separator (vapor-liquid-liquid) and two 2-phase separators (vapor-liquid & liquid-liquid) in order to select separation configuration with better performance. The process optimization on reactor and phase separator is carried out to find the operating conditions and feed conditions that can reach the maximum SO2 conversion and the minimum H2SO4 impurities in HIX phase. For reactor optimization, the maximum 98% SO2 conversion was obtained with fixed iodine and water inlet flow rate when the diameter and length of PFR reactor are 0.20 m and 7.6m. Inlet water and iodine flow rate is reduced by 17% and 22% to reach the maximum 10% SO2 conversion with fixed temperature and PFR size (diameter: 3/8", length:3 m). When temperature (121℃) and PFR size (diameter: 0.2, length:7.6 m) are applied to the feed composition optimization, inlet water and iodine flow rate is reduced by 17% and 22% to reach the maximum 10% SO2 conversion.

Validation of Onen's Alternative Grading System for Congenital Hydronephrosis (선천성 수신증을 위한 Onen 등급 분류법의 임상적인 타당성)

  • Woo, Da Eun;Lim, Myung Hee;Kim, Myung Uk;Kim, Sae Yoon;Park, Yong Hoon
    • Childhood Kidney Diseases
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    • v.18 no.2
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    • pp.77-84
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    • 2014
  • Purpose: The purpose of this study was to compare the validity of Onen's alternative grading system (AGS) with that of the APDRP and SFU grading systems in patients with isolated and complicated congenital hydronephrosis. Methods: We retrospectively reviewed the medical records of 153 patients (204 renal units) diagnosed with congenital hydronephrosis between January 2002 and December 2011. We classified patients into 2 groups; isolated or complicated hydronephrosis. All renal units were graded according to anterior-posterior diameter of renal pelvis (APDRP), Society for Fetus Urology (SFU) and Onen's grading systems. We analyzed the prognosis of hydronephrosis, according to each grading system, at 2 years of age. Results: There were 152 renal units with isolated hydronephrosis and 52 renal units with complicated hydronephrosis. The isolated hydronephrosis group had a lower grade according to Onen's AGS, and showed more frequent spontaneous remission by 2 years of age. There was more frequent obstruction (P =0.000) and surgical treatment (P =0.000) of units with high-grade hydronephrosis according to Onen's AGS. In the complicated hydronephrosis group the frequencies of spontaneous remission (P =0.015) and renal dysfunction (P =0.013) were significantly higher than those in high-grade hydronephrosis, as indicated by Onen's AGS. There were no significant differences in clinical outcomes among the highest grade groups, according to the 3 systems, in either isolated or complicated hydronephrosis. Conclusion: Onen's AGS reflects the prognosis of hydronephrosis as well as other grading systems in those with isolated hydronephrosis. It was better predictor of renal dysfunction in those with complicated hydronephrosis. However, Onen's AGS was not superior to the other grading systems in terms of predicting prognosis, especially in high-grade hydronephrosis.

Development of Rapid Analytical Method of Forbidden Medicines in Dietary Supplements Using LC-ESI-Tandem MS (LC-ESI-tandem MS를 이용한 기능성표방식품 중 부정유해물질 신속검사체계 개발)

  • Kim, Hee-Yun;Jang, Young-Mi;Joo, Hyun-Jin;Jung, Young-Hyun;Lee, Myoung-Sook;Park, Jong-Seok;Lee, Kwang-Ho;Lee, Hwa-Mi
    • Korean Journal of Food Science and Technology
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    • v.39 no.4
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    • pp.372-379
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    • 2007
  • A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

A Study on the Development of a Simulation Model for Predicting Soil Moisture Content and Scheduling Irrigation (토양수분함량 예측 및 계획관개 모의 모형 개발에 관한 연구(I))

  • 김철회;고재군
    • Magazine of the Korean Society of Agricultural Engineers
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    • v.19 no.1
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    • pp.4279-4295
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    • 1977
  • Two types of model were established in order to product the soil moisture content by which information on irrigation could be obtained. Model-I was to represent the soil moisture depletion and was established based on the concept of water balance in a given soil profile. Model-II was a mathematical model derived from the analysis of soil moisture variation curves which were drawn from the observed data. In establishing the Model-I, the method and procedure to estimate parameters for the determination of the variables such as evapotranspirations, effective rainfalls, and drainage amounts were discussed. Empirical equations representing soil moisture variation curves were derived from the observed data as the Model-II. The procedure for forecasting timing and amounts of irrigation under the given soil moisture content was discussed. The established models were checked by comparing the observed data with those predicted by the model. Obtained results are summarized as follows: 1. As a water balance model of a given soil profile, the soil moisture depletion D, could be represented as the equation(2). 2. Among the various empirical formulae for potential evapotranspiration (Etp), Penman's formula was best fit to the data observed with the evaporation pans and tanks in Suweon area. High degree of positive correlation between Penman's predicted data and observed data with a large evaporation pan was confirmed. and the regression enquation was Y=0.7436X+17.2918, where Y represents evaporation rate from large evaporation pan, in mm/10days, and X represents potential evapotranspiration rate estimated by use of Penman's formula. 3. Evapotranspiration, Et, could be estimated from the potential evapotranspiration, Etp, by introducing the consumptive use coefficient, Kc, which was repre sensed by the following relationship: Kc=Kco$.$Ka+Ks‥‥‥(Eq. 6) where Kco : crop coefficient Ka : coefficient depending on the soil moisture content Ks : correction coefficient a. Crop coefficient. Kco. Crop coefficients of barley, bean, and wheat for each growth stage were found to be dependent on the crop. b. Coefficient depending on the soil moisture content, Ka. The values of Ka for clay loam, sandy loam, and loamy sand revealed a similar tendency to those of Pierce type. c. Correction coefficent, Ks. Following relationships were established to estimate Ks values: Ks=Kc-Kco$.$Ka, where Ks=0 if Kc,=Kco$.$K0$\geq$1.0, otherwise Ks=1-Kco$.$Ka 4. Effective rainfall, Re, was estimated by using following relationships : Re=D, if R-D$\geq$0, otherwise, Re=R 5. The difference between rainfall, R, and the soil moisture depletion D, was taken as drainage amount, Wd. {{{{D= SUM from { {i }=1} to n (Et-Re-I+Wd)}}}} if Wd=0, otherwise, {{{{D= SUM from { {i }=tf} to n (Et-Re-I+Wd)}}}} where tf=2∼3 days. 6. The curves and their corresponding empirical equations for the variation of soil moisture depending on the soil types, soil depths are shown on Fig. 8 (a,b.c,d). The general mathematical model on soil moisture variation depending on seasons, weather, and soil types were as follow: {{{{SMC= SUM ( { C}_{i }Exp( { - lambda }_{i } { t}_{i } )+ { Re}_{i } - { Excess}_{i } )}}}} where SMC : soil moisture content C : constant depending on an initial soil moisture content $\lambda$ : constant depending on season t : time Re : effective rainfall Excess : drainage and excess soil moisture other than drainage. The values of $\lambda$ are shown on Table 1. 7. The timing and amount of irrigation could be predicted by the equation (9-a) and (9-b,c), respectively. 8. Under the given conditions, the model for scheduling irrigation was completed. Fig. 9 show computer flow charts of the model. a. To estimate a potential evapotranspiration, Penman's equation was used if a complete observed meteorological data were available, and Jensen-Haise's equation was used if a forecasted meteorological data were available, However none of the observed or forecasted data were available, the equation (15) was used. b. As an input time data, a crop carlender was used, which was made based on the time when the growth stage of the crop shows it's maximum effective leaf coverage. 9. For the purpose of validation of the models, observed data of soil moiture content under various conditions from May, 1975 to July, 1975 were compared to the data predicted by Model-I and Model-II. Model-I shows the relative error of 4.6 to 14.3 percent which is an acceptable range of error in view of engineering purpose. Model-II shows 3 to 16.7 percent of relative error which is a little larger than the one from the Model-I. 10. Comparing two models, the followings are concluded: Model-I established on the theoretical background can predict with a satisfiable reliability far practical use provided that forecasted meteorological data are available. On the other hand, Model-II was superior to Model-I in it's simplicity, but it needs long period and wide scope of observed data to predict acceptable soil moisture content. Further studies are needed on the Model-II to make it acceptable in practical use.

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Simultaneous Determination of Water Soluble Vitamins B Group in Health Functional Foods etc. by HPLC (건강기능식품 등 중 수용성 비타민 B군의 HPLC를 이용한 동시분석법)

  • Kim, Seon Hee;Kim, Jae-Hyun;Lee, Hwa Jung;Oh, Jae Myoung;Lee, Sung Hye;Bahn, Kyeong Nyeo;Seo, Il Won;Lee, Young Joo;Lee, Jin Hee;Kang, Tae Seok
    • Journal of Food Hygiene and Safety
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    • v.30 no.2
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    • pp.143-149
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    • 2015
  • This study was conducted to simultaneous analysis methods for water soluble vitamins B group (vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$) which is used as health functional foods etc. Analytical methods of water-soluble vitamins B group by HPLC were established through instrumental analytical conditions, and the examination of data such as domestic and foreign reliable methods, and papers of journal. HPLC method analyzing water soluble vitamins B group was established using Capcell Pak C18 UG 120 column in 270 nm through test of columns. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for water soluble vitamins B group. An excellent linearity ($r^2=0.999$) was observed for vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$ in the concentration range ($0.1{\sim}2{\mu}g/mL$). Observed recovery of vitamin $B_1$ was found to be between 100 and 103%, vitamin $B^2$ was found to be between 104 and 112%, nicotinic acid was found to be between 82 and 85%, nicotinamide was found to be between 121 and 124% and vitamin $B_6$ was found to be between 95 and 104%. LOQ of vitamin $B_1$ was found to be $0.04{\mu}g/mL$, vitamin $B_2$ was found to be $0.05{\mu}g/mL$, nicotinic acid was found to be $0.15{\mu}g/mL$, nicotinamide was found to be $0.08{\mu}g/mL$ and vitamin $B_6$ was found to be $0.63{\mu}g/mL$. Repeatability precision for vitamin $B_1$ was found to be 0.4%, vitamin $B_2$ was found to be 0.4%, nicotinic acid was found to be 0.5%, nicotinamide was found to be 0.7% and vitamin $B_6$ was found to be 0.4% relative standard deviation (RSD). Also, verify the accuracy of the simultaneous analysis methods, we monitored the labeled contents of the health functional foods and children's preferred foods.