• Title/Summary/Keyword: Calibration & Validation

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The Alignment Evaluation for Patient Positioning System(PPS) of Gamma Knife PerfexionTM (감마나이프 퍼펙션의 자동환자이송장치에 대한 정렬됨 평가)

  • Jin, Seong Jin;Kim, Gyeong Rip;Hur, Beong Ik
    • Journal of the Korean Society of Radiology
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    • v.14 no.3
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    • pp.203-209
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    • 2020
  • The purpose of this study is to assess the mechanical stability and alignment of the patient positioning system (PPS) of Leksell Gamma Knife Perfexion(LGK PFX). The alignment of the PPS of the LGK PFX was evaluated through measurements of the deviation of the coincidence of the Radiological Focus Point(RFP) and the PPS Calibration Center Point(CCP) applying different weights on the couch(0, 50, 60, 70, 80, and 90 kg). In measurements, a service diode test tool with three diode detectors being used biannually at the time of the routine preventive maintenance was used. The test conducted with varying weights on the PPS using the service diode test tool measured the radial deviations for all three collimators 4, 8, and 16 mm and also for three different positions of the PPS. In order to evaluate the alignment of the PPS, the radial deviations of the correspondence of the radiation focus and the LGK calibration center point of multiple beams were averaged using the calibrated service diode test tool at three university hospitals in Busan and Gyeongnam. Looking at the center diode for all collimators 4, 8, and 16 mm without weight on the PPS, and examining the short and long diodes for the 4 mm collimator, the means of the validation difference, i.e., the radial deviation for the setting of 4, 8, and 16 mm collimators for the center diode were respectively measured to 0.058 ± 0.023, 0.079 ± 0.023, and 0.097 ± 0.049 mm, and when the 4 mm collimator was applied to the center diode, the short diode, and the long diode, the average of the radial deviation was respectively 0.058 ± 0.023, 0.078 ± 0.01 and 0.070 ± 0.023 mm. The average of the radial deviations when irradiating 8 and 16 mm collimators on short and long diodes without weight are measured to 0.07 ± 0.003(8 mm sd), 0.153 ± 0.002 mm(16 mm sd) and 0.031 ± 0.014(8 mm ld), 0.175 ± 0.01 mm(16 mm ld) respectively. When various weights of 50 to 90 kg are placed on the PPS, the average of radial deviation when irradiated to the center diode for 4, 8, and 16 mm is 0.061 ± 0.041 to 0.075 ± 0.015, 0.023 ± 0.004 to 0.034 ± 0.003, and 0.158 ± 0.08 to 0.17 ± 0.043 mm, respectively. In addition, in the same situation, when the short diode for 4, 8, and 16 mm was irradiated, the averages of radial deviations were 0.063 ± 0.024 to 0.07 ± 0.017, 0.037 ± 0.006 to 0.059 ± 0.001, and 0.154 ± 0.03 to 0.165 ± 0.07 mm, respectively. In addition, when irradiated on long diode for 4, 8, and 16 mm, the averages of radial deviations were measured to be 0.102 ± 0.029 to 0.124 ± 0.036, 0.035 ± 0.004 to 0.054 ± 0.02, and 0.183 ± 0.092 to 0.202 ± 0.012 mm, respectively. It was confirmed that all the verification results performed were in accordance with the manufacturer's allowable deviation criteria. It was found that weight dependence was negligible as a result of measuring the alignment according to various weights placed on the PPS that mimics the actual treatment environment. In particular, no further adjustment or recalibration of the PPS was required during the verification. It has been confirmed that the verification test of the PPS according to various weights is suitable for normal Quality Assurance of LGK PFX.

Development of Analytical Method for Detection of Fungicide Validamycin A Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Validamycin A의 시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.22-29
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    • 2019
  • Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

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.

Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.161-170
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    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

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.

Non Destructive Fast Determination of Fatty Acid Composition by Near Infrared Reflectance Spectroscopy in Sesame

  • Kang, Churl-Whan;Kim, Dong-Hwi;Lee, Sung-Woo;Kim, Ki-Jong;Cho, Kyu-Chae;Shim, Kang-Bo
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.51 no.spc1
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    • pp.283-291
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    • 2006
  • To investigate seed non destructive and fast determination technique utilizing near infrared reflectance spectroscopy (NIRs) for screening ultra high oleic (C18:1) and linoleic (C18:2) fatty acid content sesame varieties among genetic resources and lines of pedigree generations of cross and mutation breeding were carried out in National Institute of Crop Science (NICS). 150 among 378 landraces and introduced cultivars were released to analyse fatty acids by NIRs and gas chromatography (GC). Average content of each fatty acid was 9.64% in palmitic acid (C16:0), 4.73% in stearic acid (C18:0), 42.26% in oleic acid and 43.38% in linoleic acid by GC. The content range of each fatty acid was from 7.29 to 12.27% in palmitic, 6.49% from 2.39 to 8.88% in stearic, 12.59% of wider range compared to that of stearic and palmitic from 37.36 to 49.95% in oleic and of the widest from 30.60 to 47.40% in linoleic acid. Spectrums analyzed by NIRs were distributed from 400 to 2,500 nm wavelengths and varietal distribution of fatty acids were appeared as regular distribution. Varietal differences of oleic acid content good for food processing and human health by NIRs was 14.08% of which 1.49% wider range than that of GC from 38.31 to 52.39%. Varietal differences of linoleic acid content by NIRs was 16.41% of which 0.39% narrower range than that of GC from 30.60 to 47.01%. Varietal differences of oleic and linoleic acid content in NIRs analysis were appeared relatively similar inclination compared with those of GC. Partial least square regression (PLSR) among multiple variant regression (MVR) in NIRs calibration statistics was carried out in spectrum characteristics on the wavelength from 700 to 2,500 nm with oleic and linoleic acids. Correlation coefficient of root square (RSQ) in oleic acid content was 0.724 of which 72.4 percent of sample varieties among all distributed in the range of 0.570 percent of standard error when calibrated (SEC) which were considerably acceptable in statistic confidence significantly for analysis between NIRs and GC. Standard error of cross validation (SECV) of oleic acid was 0.725 of which distributed in the range of 0.725 percent standard error among the samples of mother population between analyzed value by NIRs analysis and analyzed value by GC. RSQ of linoleic acid content was 0.735 of which 73.5 percent of sample varieties among all distributed in the range of 0.643 percent of SEC. SECV of linoleic acid was 0.711 of which distributed in the range of 0.711 percent standard error among the samples of mother population between NIRs analysis and GC analysis. Consequently, adoption NIR analysis for fatty acids of oleic and linoleic instead that of GC was recognized statistically significant between NIRs and GC analysis through not only majority of samples distributed in the range of negligible SEC but also SECV. For enlarging and increasing statistic significance of NIRs analysis, wider range of fatty acids contented sesame germplasm should be kept on releasing additionally for increasing correlation coefficient of RSQ and reducing SEC and SECV in the future.

Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC (Macrolide계 항생물질 동시분석법 확립 및 모니터링)

  • Park, Sang-Ouk;Lee, Sang-Ho;Ahn, Jong-Hoon;Jung, Young-Ji;Kim, Seong-Cheol;Kim, Ji-Yeon;Keum, Eun-Hee;Sung, Ju-Hyun;Kim, Sang-Yub;Jang, Young-Mi;Kang, Chan-Soon
    • Korean Journal of Food Science and Technology
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    • v.42 no.3
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    • pp.287-291
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    • 2010
  • In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.

DISEASE DIAGNOSED AND DESCRIBED BY NIRS

  • Tsenkova, Roumiana N.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1031-1031
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    • 2001
  • The mammary gland is made up of remarkably sensitive tissue, which has the capability of producing a large volume of secretion, milk, under normal or healthy conditions. When bacteria enter the gland and establish an infection (mastitis), inflammation is initiated accompanied by an influx of white cells from the blood stream, by altered secretory function, and changes in the volume and composition of secretion. Cell numbers in milk are closely associated with inflammation and udder health. These somatic cell counts (SCC) are accepted as the international standard measurement of milk quality in dairy and for mastitis diagnosis. NIR Spectra of unhomogenized composite milk samples from 14 cows (healthy and mastitic), 7days after parturition and during the next 30 days of lactation were measured. Different multivariate analysis techniques were used to diagnose the disease at very early stage and determine how the spectral properties of milk vary with its composition and animal health. PLS model for prediction of somatic cell count (SCC) based on NIR milk spectra was made. The best accuracy of determination for the 1100-2500nm range was found using smoothed absorbance data and 10 PLS factors. The standard error of prediction for independent validation set of samples was 0.382, correlation coefficient 0.854 and the variation coefficient 7.63%. It has been found that SCC determination by NIR milk spectra was indirect and based on the related changes in milk composition. From the spectral changes, we learned that when mastitis occurred, the most significant factors that simultaneously influenced milk spectra were alteration of milk proteins and changes in ionic concentration of milk. It was consistent with the results we obtained further when applied 2DCOS. Two-dimensional correlation analysis of NIR milk spectra was done to assess the changes in milk composition, which occur when somatic cell count (SCC) levels vary. The synchronous correlation map revealed that when SCC increases, protein levels increase while water and lactose levels decrease. Results from the analysis of the asynchronous plot indicated that changes in water and fat absorptions occur before other milk components. In addition, the technique was used to assess the changes in milk during a period when SCC levels do not vary appreciably. Results indicated that milk components are in equilibrium and no appreciable change in a given component was seen with respect to another. This was found in both healthy and mastitic animals. However, milk components were found to vary with SCC content regardless of the range considered. This important finding demonstrates that 2-D correlation analysis may be used to track even subtle changes in milk composition in individual cows. To find out the right threshold for SCC when used for mastitis diagnosis at cow level, classification of milk samples was performed using soft independent modeling of class analogy (SIMCA) and different spectral data pretreatment. Two levels of SCC - 200 000 cells/$m\ell$ and 300 000 cells/$m\ell$, respectively, were set up and compared as thresholds to discriminate between healthy and mastitic cows. The best detection accuracy was found with 200 000 cells/$m\ell$ as threshold for mastitis and smoothed absorbance data: - 98% of the milk samples in the calibration set and 87% of the samples in the independent test set were correctly classified. When the spectral information was studied it was found that the successful mastitis diagnosis was based on reviling the spectral changes related to the corresponding changes in milk composition. NIRS combined with different ways of spectral data ruining can provide faster and nondestructive alternative to current methods for mastitis diagnosis and a new inside into disease understanding at molecular level.

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Analysis of Diflubenzuron in Agricultural Commodities by Multiresidue Method (동시 다성분 분석법에 의한 농산물 중 Diflubenzuron 분석)

  • Park, Sun-Hee;Han, Chang-Ho;Kim, Ae-Kyung;Shin, Jae-Min;Lee, Jae-Kyoo;Park, Young-Hae;Kim, Ji-Min;Hwang, Lae-Hong;Chang, Min-Su;Song, Mi-Ok;Park, Ju-Sung;Yun, Eun-Sun;Kim, Mu-Sang;Jung, Kweon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.269-277
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    • 2014
  • The multiclass pesticide multiresidue method for the simultaneous determination of diflubenzuron in agricultural products was conducted by using HPLC-UVD. The method was validated through the guidelines of linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision with pesticide-free spinach, Korean cabbage, eggplant, squash, sweet pepper, cucumber, Korean melon. The calibration curve of diflubenzuron was linear over the concentration range of 0.05-5 mg/kg with correlation coefficient of above 0.99999. The limit of detection and quantification was 0.008 and 0.02 mg/kg. Mean recoveries of diflubenzuron for each sample were 77.5-105.6%. Relative standard deviation (RSD) in recoveries were all less than 20%. The intra-day and inter-day precision (RSD) were 0.4-1.9% and 0.7-1.9%, respectively. The result of validation indicated that this method was accurate and rapid assay.

Improvement of Mid-and Low-flow Estimation Using Variable Nonlinear Catchment Wetness Index (비선형 유역습윤지수를 이용한 평갈수기 유출모의개선)

  • Hyun, Sukhoon;Kang, Boosik;Kim, Jin-Gyeom
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.36 no.5
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    • pp.779-789
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    • 2016
  • The effective rainfall is calculated considering the soil moisture. It utilizes observed data directly in order to incorporate the soil moisture into the rainfall-runoff model, or it calculates indirectly within the model. The rainfall-runoff model, IHACRES, used in this study computes the catchment wetness index (CWI) first varying with temperature and utilize it for estimating precipitation loss. The nonlinear relationship between the CWI and the effective rainfall in the Hapcheondam watershed was derived and utilized for the long-term runoff calculation. The effects of variable and constant CWI during calibration and validation were suggested by flow regime. The results show the variable CWI is generally more effective than the constant CWI. The $R^2$ during high flow period shows relatively higher than the ones during normal or low flow period, but the difference between cases of the variable and constant CWI was insignificant. The results indicates that the high flow is relatively less sensitive to the evaporation and soil moisture associated with temperature. On the other hand, the variable CWI gives more desirable results during normal and low flow periods which means that it is crucial to incorporate evaporation and soil moisture depending on temperature into long-term continuous runoff simulation. The NSE tends to decrease during high flow period with high variability which could be natural because NSE index is largely influenced by outliers of underlying variable. Nevertheless overall NSE shows satisfactory range higher than 0.9. The utilization of variable CWI during normal and low flow period would improve the computation of long-term rainfall-runoff simulation.