• Title/Summary/Keyword: calibration coefficients

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Determination of Nitrovin in Fishery Products by Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS를 이용한 수산물 중 니트로빈의 정량분석법 개발 및 검증)

  • Kim, Joohye;Shin, Dasom;Kang, Hui-Seung;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.33 no.2
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    • pp.118-123
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    • 2018
  • The objective of this study was to develop a sensitive method for the identification and determination of nitrovin in fishery products by using a solid-phase extraction (SPE), as performed with a liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with a mixture of acetonitrile and water, and were then defatted with acetonitrile saturated hexane, after which further clean-up was accomplished with SPE on the hydrophilic-lipophilic balance (HLB) cartridges. The analytes were subsequently ionized in the positive mode of an electrospray ionization (ESI), and where thereby detected in a process of multiple reaction monitoring (MRM). The linearity (expressed as correlation coefficients) of the matrix calibration curves was > 0.985. The limit of the quantification for the nitrovin was measured at 0.001 mg/kg. The accuracy (expressed as average recovery) was noted between 72.1 and 122%. The precision (expressed as coefficient variation) was noted from 2.9 to 16.9%. According to the CODEX CAC/GL-71 guideline accuracy, precision, linearity, and limit of detection were determined in three matrices (which were flatfish, eel and shrimp). The proposed method was suitable for analyzing the associated nitrovin residues. This application and result can also be a factor to contribute to the non-detection drugs management in fishery products.

Validation and Uncertainty Evaluation of an Optimized Analytical Method Using HPLC Applied to Canthaxanthin, a Food Colorant (식품 색소 Canthaxanthin의 HPLC 최적 분석법 확인 및 타당성과 측정불확도 평가)

  • Suh, Hee-Jae;Kim, Kyung-Su;Hong, Mi-Na;Lee, Chan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.3
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    • pp.342-351
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    • 2016
  • This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

Development the Geostationary Ocean Color Imager (GOCI) Data Processing System (GDPS) (정지궤도 해색탑재체(GOCI) 해양자료처리시스템(GDPS)의 개발)

  • Han, Hee-Jeong;Ryu, Joo-Hyung;Ahn, Yu-Hwan
    • Korean Journal of Remote Sensing
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    • v.26 no.2
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    • pp.239-249
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    • 2010
  • The Geostationary Ocean Color Imager (GOCI) data-processing system (GDPS), which is a software system for satellite data processing and analysis of the first geostationary ocean color observation satellite, has been developed concurrently with the development of th satellite. The GDPS has functions to generate level 2 and 3 oceanographic analytical data, from level 1B data that comprise the total radiance information, by programming a specialized atmospheric algorithm and oceanic analytical algorithms to the software module. The GDPS will be a multiversion system not only as a standard Korea Ocean Satellite Center(KOSC) operational system, but also as a basic GOCI data-processing system for researchers and other users. Additionally, the GDPS will be used to make the GOCI images available for distribution by satellite network, to calculate the lookup table for radiometric calibration coefficients, to divide/mosaic several region images, to analyze time-series satellite data. the developed GDPS system has satisfied the user requirement to complete data production within 30 minutes. This system is expected to be able to be an excellent tool for monitoring both long-term and short-term changes of ocean environmental characteristics.

Validation on the Analytical Method of Ginsenosides in Red Ginseng

  • Cho B. G.;Nho K. B.;Shon H. J.;Choi K. J.;Lee S. K.;Kim S. C;Ko S. R.;Xie P. S.;Yan Y. Z.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.491-501
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    • 2002
  • A cross-examination between KT&G Central Research Institute and Guangzhou Institute for Drug Control was carried out in order to select optimum conditions for extraction, separation and determination of ginsenosides in red ginseng and to propose a better method for the quantitative analysis of ginsenosides. The optimum extraction conditions of ginsenosides from red ginseng were as follows: the extraction solvent, $70\%$ methanol; the extraction temperature, $100^{\circ}C;$ the extraction time, 1 hour for once; and the repetition of extraction, twice. The optimum separation conditions of ginsenosides on the SepPak $C_{18}$ cartridge were as follows: the loaded amount, 0.4 g of methanol extract; the washing solvents, distilled water of 25 ml at first and then $30\%$ methanol of 25 ml; the elution solvent, $90\%$ methanol of 5 ml. The optimum HPLC conditions for the determination of ginsenosides were as follows: column, Lichrosorb $NH_2(25{\times}0.4cm,$ 5${\mu}m$, Merck Co.); mobile phase, a mixture of acetonitrile/water/isopropanol (80/5/15) and acetonitrile/water/isopropanol (80/20/15) with gradient system; and the detector, ELSD. On the basis of the optimum conditions a method for the quantitative analysis of ginsenosides were proposed and another cross-examination was carried out for the validation of the selected analytical method conditions. The coefficient of variances (CVs) on the contents of ginsenoside-$Rg_{1}$, -Re and $-Rb_1$ were lower than $3\%$ and the recovery rates of ginsenosides were $89.4\~95.7\%,$ which suggests that the above extraction and separation conditions may be reproducible and reasonable. For the selected HPLC/ELSD conditions, the CVs on the detector responses of ginsenoside-Rg, -Re and $-Rb_1$) were also lower than $3\%$, the regression coefficients for the calibration curves of ginsenosides were higher than 0.99 and two adjacent ginsenoside peaks were well separated, which suggests that the above HPLC/ELSD conditions may be good enough for the determination of ginsenosides.

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Development and Validation of an Analytical Method for β-Agonists in Livestock and Fishery Products Using LC-MS/MS (LC-MS/MS를 이용한 축·수산물 중 β-agonist계 시험법 개발 및 검증)

  • Lee, Tae Ho;Kim, Yu Ra;Park, Su Jeong;Kim, Ji Young;Choi, Jang Duck;Moon, Gui Im
    • Korean Journal of Environmental Agriculture
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    • v.41 no.2
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    • pp.135-151
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    • 2022
  • BACKGROUND: The β-agonists known as phenyl ethanolamine derivatives have a conjugated aromatic ring with amino group. They are used as tocolytic agents and bronchodilator to human and animal generally, and some of them are used as growth promoters to livestock. METHODS AND RESULTS: β-agonists in samples were extracted by 0.4 N perchloric acid and ethyl acetate. The target compounds were analyzed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS). Validation of method was performed according to CODEX guidelines (CAC/GL-71). The matrix matched calibration gave correlation coefficients>0.98, and the obtained recoveries were in the range of 62.0-109.8%, with relative standard deviation ≤ 20.1%. In addition, a survey was performed to inspect any residual β-agonist from 100 samples of livestock and fishery products and ractopamine was detected in one of the 100 samples. CONCLUSION(S): In this study, we established the analytical method for β-agonists through using the expanded target compounds and samples. And we anticipate that the established method would be used for analysis to determine veterinary drug residues in livestock and fishery products.

Development of the Simultaneous Analysis of 36 Sulfonylurea Herbicide Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 제초제 Sulfonylurea계 36종 동시 시험법 개발)

  • Su Jung Lee;Jung Mi Lee;Gui Hyun Jang;Hyun-Kyung Kim;Ji Young Kim
    • Korean Journal of Environmental Agriculture
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    • v.42 no.2
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    • pp.139-151
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    • 2023
  • Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO4 and C18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R2) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

Determination of thyroid hormones in plasma samples by high performance liquid chromatograph/diode array detector/electrospray ionization mass spectrometer (HPLC/DAD/ESI-MS를 이용한 혈장시료 중 갑상선 호르몬 분석)

  • Kwak, Sun Young;Moon, Myeong Hee;Pyo, Heesoo
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.424-433
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    • 2007
  • An analytical method for the determination of thyroid hormones in plasma samples has been studied by solid-phase extraction and high-performance liquid chromatography/diode array detector (DAD)/electrospray ionization (ESI)-mass spectrometer. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 250 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile. In addition, these compounds were confirmed by UV spectra and ESI-mass Spectra. The extraction recoveries of thyroid hormones in the plasma sample (at pH 3) were in the range of 74.5-115.7 % with solid-phase extraction by C18, followed by elution with 4 mL of methanol. The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.9939 to 0.9978 and the detection limits of all analytes were obtained in the range of 20-50 ng/mL (38.1-162.8 pmol/mL). As a result, thyroxine was found in the range of 50.98-112.97 ng/mL in normal plasma samples.

Simultaneous analysis of residual glucocorticoids in egg by LC/MS/MS (LC/MS/MS를 이용한 계란 중 잔류 글루코코티코이드의 동시분석)

  • Jang, Mi-Ae;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.326-335
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    • 2009
  • A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

Parameter Calibration of Storage Function Model and Flood Forecasting (2) Comparative Study on the Flood Forecasting Methods (저류함수모형의 매개변수 보정과 홍수예측 (2) 홍수예측방법의 비교 연구)

  • Kim, Bum Jun;Song, Jae Hyun;Kim, Hung Soo;Hong, Il Pyo
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.26 no.1B
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    • pp.39-50
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    • 2006
  • The flood control offices of main rivers have used a storage function model to forecast flood stage in Korea and studies of flood forecasting actively have been done even now. On this account, the storage function model, which is used in flood control office, regression models and artificial neural network model are applied into flood forecasting of study watershed in this paper. The result obtained by each method are analyzed for the comparative study. In case of storage function model, this paper uses the representative parameters of the flood control offices and the optimized parameters. Regression coefficients are obtained by regression analysis and neural network is trained by backpropagation algorithm after selecting four events between 1995 to 2001. As a result of this study, it is shown that the optimized parameters are superior to the representative parameters for flood forecasting. The results obtained by multiple, robust, stepwise regression analysis, one of the regression methods, show very good forecasts. Although the artificial neural network model shows less exact results than the regression model, it can be efficient way to produce a good forecasts.

Calibration of Hargreaves Equation Coefficient for Estimating Reference Evapotranspiration in Korea (우리나라 기준증발산량 추정을 위한 Hargreaves 공식의 계수 보정)

  • Hwang, Seon-ah;Han, Kyung-hwa;Zhang, Yong-seon;Cho, Hee-rae;Ok, Jung-hun;Kim, Dong-Jin;Kim, Gi-sun;Jung, Kang-ho
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.21 no.4
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    • pp.238-249
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    • 2019
  • The evapotranspiration is estimated based on weather factors such as temperature, wind speed and humidity, and the Hargreaves equation is a simple equation for calculating evapotranspiration using temperature data. However, the Hargreaves equation tends to be underestimated in areas with wind speeds above 3 m s-1 and overestimated in areas with high relative humidity. The study was conducted to determine Hargreaves equation coefficient in 82 regions in Korea by comparing evapotranspiration determined by modified Hargreaves equation and the Penman-Monteith equation for the time period of 2008~2018. The modified Hargreaves coefficients for 50 inland areas were estimated to be 0.00173~0.00232(average 0.00196), which is similar to or lower than the default value 0.0023. On the other hand, there are 32 coastal areas, and the modified coefficients ranged from 0.00185 to 0.00303(average 0.00234). The east coastal area was estimated to be similar to or higher than the default value, while the west and south coastal areas showed large deviations by area. As results of estimating the evapotranspiration by the modified Hargreaves coefficient, root mean square error(RMSE) is reduced from 0.634~1.394(average 0.857) to 0.466~1.328(average 0.701), and Nash-Sutcliffe Coefficient(NSC) increased from -0.159~0.837(average 0.647) to -0.053~0.910(average 0.755) compared with original Hargreaves equation. Therefore, we confirmed that the Hargreaves equation can be overestimated or underestimated compared to the Penman-Monteith equation, and expected that it will be able to calculate the high accuracy evapotranspiration using the modified Hargreaves equation. This study will contribute to water resources planning, irrigation schedule, and environmental management.