• Title/Summary/Keyword: method validation

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Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증)

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via 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 (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Validation of a Method and Evaluation of Antioxidant Activity for the Simultaneous Determination of Riboflavin and Coixol in Coix lacryma-jobi var. ma-yuen Stapf Sprouts (율무 새싹 추출물의 Riboflavin과 Coixol의 동시 분석법 검증 및 항산화 활성)

  • Lee, Ji Yeon;Park, Jung Yong;Park, Chun-Geon;Kim, Dong Hwi;Ji, Yun-Jeong;Choi, Su Ji;Oh, MyeongWon;Hwang, Hosop;Lee, Yunji;Jeong, Jintae;Lee, Jeong Hoon;Seo, Kyung Hye
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.64 no.4
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    • pp.452-458
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    • 2019
  • Coix lacryma-jobi var. ma-yuen (Rom. Caill.) Stapf (CL), which contains riboflavin and coixol, has traditionally been used to treat cancer and arthritis. However, no method for the simultaneous determination of riboflavin and coixol in CL sprouts has been established. In this study, we established and validated a high-performance liquid chromatography-diode array detection (HPLC-DAD) method for the identification and quantification of two reference markers, riboflavin and coixol, in CL sprout extracts. CL sprouts (whole sprouts and leaves) were subjected to extraction with 70% ethanol at room temperature and at 80 ℃ under reflux conditions. The two extractions were validated with respect to specificity, accuracy, precision, and linearity. The content of the two reference markers was highest in leaves extracted under reflux conditions (riboflavin, 8.23 ± 0.32 mg/g; coixol, 5.95 ± 0.04 mg/g). We also investigated the antioxidant activity of the extracts via 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS+) scavenging assays. The results indicated that extracts obtained from sprouts under reflux conditions had the strongest antioxidative effects (DPPH half maximal inhibitory concentration [IC50], 68.9 ± 4.1 g/mL; and ABTS, IC50, 34.9 ± 0.1 g/mL). These results can serve as baseline data for the simultaneous determination of the two reference marker compounds, riboflavin and coixol, and development of functional food materials using CL sprouts.

A Study on Phthalate Analysis of Nail Related Products (네일 관련 제품들의 프탈레이트 분석에 관한 연구)

  • Rark, Sin-Hee;Song, Seo-Hyeon;Kim, Hyun-Joo;Cho, Youn-Sik;Kim, Ae-Ran;Kim, Beom-Ho;Hong, Mi-Yeun;Park, Sang-Hyun;Yoon, Mi-Hye
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.45 no.3
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    • pp.217-224
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    • 2019
  • Phthalates, endocrine disrupting chemicals, are similar in structure to sex hormones and mainly show reproductive toxicity and developmental toxicity. In this study, we analyzed 11 phthalates, including 3 kinds of phthalates prohibited in cosmetic use and 8 kinds of phthalates regulated in 'Common standards for children's products safety' and EU cosmetic regulation (EC No. 1223/2009). The phthalate analysis was optimized using GC-MS/MS. In analytical method validation, this method was satisfied in specificity, linearity, recovery rate, accuracy and MQL. Therefore, we used this method to analyze 82 products of Nail cosmetics & polish. Although six phthalates such as DBP, BBP, DEHP, DPP, DIBP and DIDP were detected at concentrations of $1.0{\sim}59.8{\mu}g/g$g, they were suitable to Korean cosmetic standards. DIBP and DBP were detected at concentration of $1.1{\sim}2.6{\mu}g/g$ in artificial nail, DBP and DEHP were $1.4{\sim}2.5{\mu}g/g$ in glue for nails, and DIBP, DBP, and DEHP were $2.5{\sim}33.3{\mu}g/g$ in nail stickers. Although substances such as DBP and DEHP in artificial nail, Glue for nails, and nail stickers were detected, they were suitable to 'Common safety standards for children's products. DIBP is not a regulated substance in Korea but showed the third highest detection rate following DBP (84.6%) and DEHP (63.4%). The concentration of phthalates detected in nail products is considered to be safe in current standards but continuous monitoring and research about non-regulated substances are also needed to be considered.

Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.259-266
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    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

Analytical Method for Determination of Laccaic Acids in Foods with HPLC-PDA and Monitoring (식품 중 락카인산 성분 분리정제를 통한 분석법 확립 및 실태조사)

  • Jae Wook Shin;Hyun Ju Lee;Eunjoo Lim;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.390-401
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    • 2023
  • Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r2=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

Optimization of Multiclass Support Vector Machine using Genetic Algorithm: Application to the Prediction of Corporate Credit Rating (유전자 알고리즘을 이용한 다분류 SVM의 최적화: 기업신용등급 예측에의 응용)

  • Ahn, Hyunchul
    • Information Systems Review
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    • v.16 no.3
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    • pp.161-177
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    • 2014
  • Corporate credit rating assessment consists of complicated processes in which various factors describing a company are taken into consideration. Such assessment is known to be very expensive since domain experts should be employed to assess the ratings. As a result, the data-driven corporate credit rating prediction using statistical and artificial intelligence (AI) techniques has received considerable attention from researchers and practitioners. In particular, statistical methods such as multiple discriminant analysis (MDA) and multinomial logistic regression analysis (MLOGIT), and AI methods including case-based reasoning (CBR), artificial neural network (ANN), and multiclass support vector machine (MSVM) have been applied to corporate credit rating.2) Among them, MSVM has recently become popular because of its robustness and high prediction accuracy. In this study, we propose a novel optimized MSVM model, and appy it to corporate credit rating prediction in order to enhance the accuracy. Our model, named 'GAMSVM (Genetic Algorithm-optimized Multiclass Support Vector Machine),' is designed to simultaneously optimize the kernel parameters and the feature subset selection. Prior studies like Lorena and de Carvalho (2008), and Chatterjee (2013) show that proper kernel parameters may improve the performance of MSVMs. Also, the results from the studies such as Shieh and Yang (2008) and Chatterjee (2013) imply that appropriate feature selection may lead to higher prediction accuracy. Based on these prior studies, we propose to apply GAMSVM to corporate credit rating prediction. As a tool for optimizing the kernel parameters and the feature subset selection, we suggest genetic algorithm (GA). GA is known as an efficient and effective search method that attempts to simulate the biological evolution phenomenon. By applying genetic operations such as selection, crossover, and mutation, it is designed to gradually improve the search results. Especially, mutation operator prevents GA from falling into the local optima, thus we can find the globally optimal or near-optimal solution using it. GA has popularly been applied to search optimal parameters or feature subset selections of AI techniques including MSVM. With these reasons, we also adopt GA as an optimization tool. To empirically validate the usefulness of GAMSVM, we applied it to a real-world case of credit rating in Korea. Our application is in bond rating, which is the most frequently studied area of credit rating for specific debt issues or other financial obligations. The experimental dataset was collected from a large credit rating company in South Korea. It contained 39 financial ratios of 1,295 companies in the manufacturing industry, and their credit ratings. Using various statistical methods including the one-way ANOVA and the stepwise MDA, we selected 14 financial ratios as the candidate independent variables. The dependent variable, i.e. credit rating, was labeled as four classes: 1(A1); 2(A2); 3(A3); 4(B and C). 80 percent of total data for each class was used for training, and remaining 20 percent was used for validation. And, to overcome small sample size, we applied five-fold cross validation to our dataset. In order to examine the competitiveness of the proposed model, we also experimented several comparative models including MDA, MLOGIT, CBR, ANN and MSVM. In case of MSVM, we adopted One-Against-One (OAO) and DAGSVM (Directed Acyclic Graph SVM) approaches because they are known to be the most accurate approaches among various MSVM approaches. GAMSVM was implemented using LIBSVM-an open-source software, and Evolver 5.5-a commercial software enables GA. Other comparative models were experimented using various statistical and AI packages such as SPSS for Windows, Neuroshell, and Microsoft Excel VBA (Visual Basic for Applications). Experimental results showed that the proposed model-GAMSVM-outperformed all the competitive models. In addition, the model was found to use less independent variables, but to show higher accuracy. In our experiments, five variables such as X7 (total debt), X9 (sales per employee), X13 (years after founded), X15 (accumulated earning to total asset), and X39 (the index related to the cash flows from operating activity) were found to be the most important factors in predicting the corporate credit ratings. However, the values of the finally selected kernel parameters were found to be almost same among the data subsets. To examine whether the predictive performance of GAMSVM was significantly greater than those of other models, we used the McNemar test. As a result, we found that GAMSVM was better than MDA, MLOGIT, CBR, and ANN at the 1% significance level, and better than OAO and DAGSVM at the 5% significance level.

Development of validated Nursing Interventions for Home Health Care to Women who have had a Caesarian Delivery (조기퇴원 제왕절개 산욕부를 위한 가정간호 표준서 개발)

  • HwangBo, Su-Ja
    • Journal of Korean Academy of Nursing Administration
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    • v.6 no.1
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    • pp.135-146
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    • 2000
  • The purpose of this study was to develope, based on the Nursing Intervention Classification (NIC) system. a set of standardized nursing interventions which had been validated. and their associated activities. for use with nursing diagnoses related to home health care for women who have had a caesarian delivery and for their newborn babies. This descriptive study for instrument development had three phases: first. selection of nursing diagnoses. second, validation of the preliminary home health care interventions. and third, application of the home care interventions. In the first phases, diagnoses from 30 nursing records of clients of the home health care agency at P. medical center who were seen between April 21 and July 30. 1998. and from 5 textbooks were examined. Ten nursing diagnoses were selected through a comparison with the NANDA (North American Nursing Diagnosis Association) classification In the second phase. using the selected diagnoses. the nursing interventions were defined from the diagnoses-intervention linkage lists along with associated activities for each intervention list in NIC. To develope the preliminary interventions five-rounds of expertise tests were done. During the first four rounds. 5 experts in clinical nursing participated. and for the final content validity test of the preliminary interventions. 13 experts participated using the Fehring's Delphi technique. The expert group evaluated and defined the set of preliminary nursing interventions. In the third phases, clinical tests were held at in a home health care setting with two home health care nurses using the preliminary intervention list as a questionnaire. Thirty clients referred to the home health care agency at P. medical center between October 1998 and March 1999 were the subjects for this phase. Each of the activities were tested using dichotomous question method. The results of the study are as follows: 1. For the ten nursing diagnoses. 63 appropriate interventions were selected from 369 diagnoses interventions links in NlC., and from 1.465 associated nursing activities. From the 63 interventions. the nurses expert group developed 18 interventions and 258 activities as the preliminary intervention list through a five-round validity test 2. For the fifth content validity test using Fehring's model for determining lCV (Intervention Content Validity), a five point Likert scale was used with values converted to weights as follows: 1=0.0. 2=0.25. 3=0.50. 4=0.75. 5=1.0. Activities of less than O.50 were to be deleted. The range of ICV scores for the nursing diagnoses was 0.95-0.66. for the nursing interventions. 0.98-0.77 and for the nursing activities, 0.95-0.85. By Fehring's method. all of these were included in the preliminary intervention list. 3. Using a questionnaire format for the preliminary intervention list. clinical application tests were done. To define nursing diagnoses. home health care nurses applied each nursing diagnoses to every client. and it was found that 13 were most frequently used of 400 times diagnoses were used. Therefore. 13 nursing diagnoses were defined as validated nursing diagnoses. Ten were the same as from the nursing records and textbooks and three were new from the clinical application. The final list included 'Anxiety', 'Aspiration. risk for'. 'Infant behavior, potential for enhanced, organized'. 'Infant feeding pattern. ineffective'. 'Infection'. 'Knowledge deficit'. 'Nutrition, less than body requirements. altered', 'Pain'. 'Parenting'. 'Skin integrity. risk for. impared' and 'Risk for activity intolerance'. 'Self-esteem disturbance', 'Sleep pattern disturbance' 4. In all. there were 19 interventions. 18 preliminary nursing interventions and one more intervention added from the clinical setting. 'Body image enhancement'. For 265 associated nursing activities. clinical application tests were also done. The intervention rate of 19 interventions was from 81.6% to 100%, so all 19 interventions were in c1uded in the validated intervention set. From the 265 nursing activities. 261(98.5%) were accepted and four activities were deleted. those with an implimentation rate of less than 50%. 5. In conclusion. 13 diagnoses. 19 interventions and 261 activities were validated for the final validated nursing intervention set.

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Improving the Usage of the Korea Meteorological Administration's Digital Forecasts in Agriculture: V. Field Validation of the Sky-condition based Lapse Rate Estimation Scheme (기상청 동네예보의 영농활용도 증진을 위한 방안: V. 하늘상태 기반 기온감률 추정기법의 실용성 평가)

  • Kim, Soo-ock;Yun, Jin I.
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.18 no.3
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    • pp.135-142
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    • 2016
  • The aim of this study was to confirm the improvement of efficiency for temperature estimation at 0600 and 1500 LST by using a simple method for estimating temperature lapse rate modulated by the amount of clouds in comparison with the case adopting the existing single temperature lapse rate ($-6.5^{\circ}C/km$ or $-9^{\circ}C/km$). A catchment of the 'Hadong Watermark2,' which includes Hadong, Gurye, and Gwangyang was selected as the area for evaluating the practicality of the temperature lapse rate estimation method. The weather data of 0600 and 1500 LST at 12 weather observation sites within the catchment were collected during the entire year of 2015. Also, the 'sky condition' of digital forecast products of KMA in 2015 ($5{\times}5km$ lattice resolution) were overlapped with the catchment of the 'Hadong Watermark2,' to calculate the spatial average value within the catchment, which were used to simulate the 0600 and 1500 LST temperature lapse rate of the catchment. The estimation errors of the temperatures at 0600 LST were ME $-0.39^{\circ}C$ and RMSE $1.45^{\circ}C$ in 2015, when applying the existing temperature lapse rate. Using the estimated temperature lapse rate, they were improved to ME $-0.19^{\circ}C$ and RMSE $1.32^{\circ}C$. At 1500 LST, the effect of the improvements found from the comparison between the existing temperature lapse rate and the estimated temperature lapse rate were minute, because the estimated lapse rate of clear days is not very different from the existing lapse rate. However, the estimation errors of the temperatures at 1500 LST during cloudy days were improved from ME $-0.69^{\circ}C$, RMSE $1.54^{\circ}C$ to ME $-0.51^{\circ}C$, RMSE $1.19^{\circ}C$.

Estimation of Soil Surface Temperature by Heat Flux in Soil (Heat flux를 이용한 토양 표면 온도 예측)

  • Hur, Seung-Oh;Kim, Won-Tae;Jung, Kang-Ho;Ha, Sang-Keon
    • Korean Journal of Soil Science and Fertilizer
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    • v.37 no.3
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    • pp.131-135
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    • 2004
  • This study was carried out for the analysis of temperature characteristics on soil surface using soil heat flux which is one of the important parameters forming soil temperature. Soil surface temperature was estimated by using the soil temperature measured at 10 cm soil depth and the soil heat flux measured by flux plate at 5 cm soil depth. There was time lag of two hours between soil temperature and soil heat flux. Temperature changes over time showed a positive correlation with soil heat flux. Soil surface temperature was estimated by the equation using variable separation method for soil surface temperature. Arithmetic mean using temperatures measured at soil surface and 10 cm depth, and soil temperature measured at 5 cm depth were compared for accuracy of the value. To validate the regression model through this comparison, F-validation was used. Usefulness of deductive regression model was admitted because intended F-value was smaller than 0.001 and the determination coefficient was 0.968. It can be concluded that the estimated surface soil temperatures obtained by variable separation method were almost equal to the measured surface soil temperature.