• Title/Summary/Keyword: Inter-calibration

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Analysis of Pencycuron in Agricultural Products by Simultaneous Determination (동시 다성분 분석법에 의한 농산물 중 펜시쿠론 분석)

  • Park, Young-Hye;Han, Chang-Ho;Kim, Ae-Kyung;Shin, Jae-Min;Lee, Jae-Kyoo;Park, Sun-Hee;Yun, Eun-Sun;Kim, Mu-Sang;Chae, Young-Zoo
    • The Korean Journal of Pesticide Science
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    • v.17 no.3
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    • pp.162-167
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    • 2013
  • An analytical method for the simultaneous determination of pencycuron in agricultural products was established by using GC-NPD. The method was validated through the guidelines of linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision. The calibration curve of pencycuron was linear over the concentration range of 0.02-2 mg/kg with correlation coefficient of above 0.9999. The limits of detection and quantification were 0.005 and 0.02 mg/kg. Mean recoveries of pencycuron for each sample were 79.6-107.5% at the level of 0.02 mg/kg and 86.4-112.1% at the level of 0.2 mg/kg and 84.0- 104.9% at the level of 1 mg/kg. Relative standard deviation (RSD) in recoveries were all less than 5%. The intra- and inter-day precision (RSD) were 1.6-3.0% and 5.3-11.5%, respectively. The result of validation indicated that this method was accurate and sensitive assay.

Comparison of Extraction Methods for Determination of Vitamin K1 in Vegetables (채소류의 비타민 K1 분석을 위한 추출방법의 비교)

  • Kim, Hyeongi;Choi, Youngmin;Cho, Young-Sook;Sung, Jeehye;Ham, Hyeonmi;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.11
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    • pp.1791-1795
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    • 2014
  • The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.

Simultaneous Determination of B Group Vitamins in Supplemented Food Products by High Performance Liquid Chromatography-Diode Array Detection

  • Suh, Joon-Hyuk;Yang, Dong-Hyug;Lee, Byung-Kyu;Eom, Han-Young;Kim, Un-Yong;Kim, Jung-Hyun;Lee, Hye-Yeon;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2648-2656
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    • 2011
  • A simple HPLC-DAD method was developed and validated to determine B group vitamin content (thiamine, riboflavin, nicotinamide, pantothenic acid, pyridoxine and folic acid) in supplemented food samples, i.e., infant formula, cereal, low-calorie food, a multi-vitamin pill and a vitamin drink. In this study, the most significant advantages were simultaneous determination of the six B group vitamins in various food matrices and a small number of sample treatment steps that required only an organic solvent, acetonitrile. Moreover, this method prevents reduction of column durability, because the mobile phase does not contain ion-pairing reagents. Analytes were separated on a Develosil RPAQUEOUS $C_{30}$ (4.6 mm ${\times}$ 250 mm, 5 ${\mu}M$ particle size) column with a gradient elution of acetonitrile and 20 mM phosphate buffer (pH 3.0) at a flow rate between 0.8 and 1.0 mL/min. Detection was performed at 275 nm, except for that of pantothenic acid (205 nm). The calibration curves for all six vitamins showed good linearity with correlation coefficients ($r^2$) higher than 0.995. The developed method was validated with respect to linearity, intra- and inter-day accuracy and precision, limit of quantification (LOQ), recovery and stability. The method showed good precision and accuracy, with intra- and inter-assay coefficients of variation less than 15% at all concentrations. The recovery was carried out according to the standard addition procedure, with yields ranging from 89.8 to 104.4%. This method was successfully applied to the determination of vitamin B groups in supplemented food products.

A CMOS Readout Circuit for Uncooled Micro-Bolometer Arrays (비냉각 적외선 센서 어레이를 위한 CMOS 신호 검출회로)

  • 오태환;조영재;박희원;이승훈
    • Journal of the Institute of Electronics Engineers of Korea SC
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    • v.40 no.1
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    • pp.19-29
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    • 2003
  • This paper proposes a CMOS readout circuit for uncooled micro-bolometer arrays adopting a four-point step calibration technique. The proposed readout circuit employing an 11b analog-to-digital converter (ADC), a 7b digital-to-analog converter (DAC), and an automatic gain control circuit (AGC) extracts minute infrared (IR) signals from the large output signals of uncooled micro-bolometer arrays including DC bias currents, inter-pixel process variations, and self-heating effects. Die area and Power consumption of the ADC are minimized with merged-capacitor switching (MCS) technique adopted. The current mirror with high linearity is proposed at the output stage of the DAC to calibrate inter-pixel process variations and self-heating effects. The prototype is fabricated on a double-poly double-metal 1.2 um CMOS process and the measured power consumption is 110 ㎽ from a 4.5 V supply. The measured differential nonlinearity (DNL) and integrat nonlinearity (INL) of the 11b ADC show $\pm$0.9 LSB and $\pm$1.8 LSB, while the DNL and INL of the 7b DAC show $\pm$0.1 LSB and $\pm$0.1 LSB.

Simultaneous Determination of Aflatoxins and Ochratoxin A in Pork by LC-MS/MS (LC-MS/MS를 이용한 돼지고기 중 총아플라톡신 및 오크라톡신 A 동시분석법 확립)

  • Paek, Ockjin;Park, Songyi;Park, Ki Hun;Kim, Sheen-Hee;Suh, Saejung;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.194-200
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    • 2016
  • Aflatoxins and ochratoxin A (AFTs and OTA) are secondary fungal metabolites produced by several moulds, mainly by Aspergillus flavus by Aspergillus ochraceus and Penicillium verrucosum, and these toxins can be transferred to animals and humans through the ingestion of contaminated feed and food. This study was to develop the analytical method for determination the levels of AFTs ($B_1$, $B_2$, $G_1$ and $G_2$) and OTA in pork. The AFTs and OTA were analyzed simultaneously by electrospray ionization in positive ion mode and mass reaction monitoring (MRM) after solid phase extract (SPE) columns clean-up. Performance characteristics, such as accuracy, precision, linear range, limit of detection (LOD) and quantification (LOQ), were also determined. Matrix-matched standard calibration was used for quantification, obtaining the recoveries in the range of 67.3~108.2% with the relative standard deviations of < 20%. Limits of detection and quantification were also estimated, obtaining the limits of quantification ranged in $0.7{\sim}1.3{\mu}g/kg$. The results of the inter-day study, which was performed with pork samples for 3 days, showed an accuracy of 92.0~109.9%. The precisions (expressed as relative standard deviation values) for the inter day variation were 2.6~17.8%. The method developed in this study was able to carry out the analysis with the satisfactory intensity and accuracy.

Validation of LC-MS/MS method for determination of ertapenem in human plasma and urine (인체 혈장 및 소변 중 에르타페넴의 정량을 위한 LC-MS/MS 분석법 검증)

  • Kim, Yun-Jeong;Han, Song-Hee;Jeon, Ji-Young;Hwang, Min-Ho;Im, Yong-Jin;Chae, Soo-Wan;Kim, Min-Gul
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.19-24
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    • 2012
  • Liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the quantitative determination of ertapenem in human plasma and urine. After addition of internal standard (ceftazidime), plasma and urine was diluted with methanol and analyzed by LC-MS/MS. Using MS/MS with multiple reaction monitoring (MRM) mode, ertapenem were selectively detected without severeinterference from human plasma and urine. The standard calibration curve for ertapenem was linear ($r^2$= 0.9996)over the concentration range 1~100 ${\mu}g/mL$ in human plasma. The intra- and inter-day precision over the concentration range of ertapenem was lower than 8.9% (correlation of variance, CV), and accuracy was between 97.2~106.2%. On the other hand, it was showed good relationship ($r^2$= 0.9992) and the precision (intra- and inter-day) over the concentration range of ertapenem was lower than CV 7.2%, and accuracy was between 97.9~111.6% for urine. This method has been successfully applied to the pharmacokinetic study of ertapenem in human plasma and urine.

Analytical Method Validation of Quercetin in Changnyeong Onion Extract as a Functional Ingredient for Functional Health Food (건강기능식품 기능성원료로서 창녕양파추출액의 지표성분 Quercetin 분석법)

  • Jeon, Seon-Young;Jeong, Eun-Jeong;Baek, Jeong-Hwa;Cha, Yong-Jun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.4
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    • pp.565-569
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    • 2011
  • Validation of quercetin as a marker compound in the standardization of Changnyeong onion extract developed for functional health food was attempted by analytical method. The specificity was satisfied with retention time and photo diode array (PDA) spectrum by analysis of quercetin using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve as coefficient of correlation ($R^2$) of 0.9986, and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.2 mg/L and 0.5 mg/L, respectively. Recovery rate test with quercetin concentration of 0.05, 0.075 and 0.1 mg/mL was revealed in the high range of 82.36~95.26%, 82.70~98.24% and 87.91~95.11%, respectively. The intra-day and inter-day precision in quercetin for Changnyeong onion extracts was 0.10~3.28% and 0.96~5.79%, respectively. Therefore, application of quercetin was validated in analytical method as a marker compound in Changnyeong onion extracts.

Flood Runoff Simulation Model by Using API (선행강우지수를 고려한 홍수유출 시뮬레이션 모형)

  • Heo, Chang-Hwan;Im, Gi-Seok;An, Gyeong-Su;Ji, Hong-Gi
    • Journal of Korea Water Resources Association
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    • v.35 no.3
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    • pp.331-344
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    • 2002
  • This study is aimed at the development of a deterministic runoff model which can be used for flood runoff. The model is formulated by the watershed runoff model. Based on the assumptions that runoff system is nonlinear, the proposed watershed runoff model is the conceptual model. In the model structure, the conceptual model divides the runoff system into a surface structure and a subsurface structure corresponding to the surface flow, and inter flow and ground water flow respectively. The lag time effect of surface can be represented by the sub-tank of surface structure in the conceptual model. The parameter calibration of inter flow and ground water flow in the subsurface structure of the conceptual model is performed by separating the components with numeric filter The runoff coefficient($\alpha$$_2$) is expressed as the function of antecedent precipitation index(API). The parameters with the surface flow can be calibrated with the runoff coefficient($\alpha$$_1$ and $\alpha$/$_{11}$) in the conceptual model. In the conceptual model, an algorithm is developed to calibrate the parameters automatically based on efficiency criteria. The comparative study shows that simulated value from the conceptual model well agreed to observed value.

Validation of an analytical method of dieckol for standardization of Ecklonia cava extract as a functional ingredient (감태추출물의 기능성원료 표준화를 위한 지표성분 dieckol의 분석법 검증)

  • Xu, Yan;Kim, Eun Suh;Lee, Ji-Soo;Kim, Gun-Hee;Lee, Hyeon Gyu
    • Korean Journal of Food Science and Technology
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    • v.51 no.5
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    • pp.420-424
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    • 2019
  • An HPLC analysis method was developed and standardized for the detection of dieckol as a functional food ingredient in Ecklonia cava extracts. HPLC was performed using a Capcell Pak C18 column ($250{\times}4.6mm$, $5{\mu}m$) with a gradient elution of water and acetonitrile, both containing 0.1% (v/v) trifluoroacetic acid, at a flow rate of 1.0 mL/min at $25^{\circ}C$. The eluate was detected at 230 nm. For validation, the specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) of dieckol were measured. The calibration curve for the detection of dieckol had high linearity ($R^2=0.9994$), with LOD and LOQ values of 0.38 and $1.16{\mu}g/mL$, respectively. Recovery of the quantified compound ranged from 99.61 to 100.71%. The relative standard deviation values of the intra-day and inter-day precisions were less than 1.7 and 1.25%, respectively. These results indicate that the reported HPLC method is simple, reliable, and reproducible for the detection of dieckol in Ecklonia cava extracts.

Development and Validation of Analytical Method for Decursin in Aerial Parts of Angelica gigas Nakai Extract (참당귀 지상부 추출물의 지표성분 decursin의 분석법 개발 및 검증)

  • Kim, Hee-Yeon;Lee, Ki-Yeon;Kim, Tae-Hee;Park, A-Reum;Noh, Hee-Sun;Kim, Si-Chang;Ahn, Mun-Seob
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.52-57
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    • 2019
  • Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column ($3{\times}150mm$, $3{\mu}m$) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9994 and the limit of detection and limit of quantitation were $0.011{\mu}g/mL$ and $0.033{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and $10{\mu}g/mL$ were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.