• Title/Summary/Keyword: Calibration Routine

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Predicting Soil Chemical Properties with Regression Rules from Visible-near Infrared Reflectance Spectroscopy

  • Hong, Suk Young;Lee, Kyungdo;Minasny, Budiman;Kim, Yihyun;Hyun, Byung Keun
    • Korean Journal of Soil Science and Fertilizer
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    • v.47 no.5
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    • pp.319-323
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    • 2014
  • This study investigates the prediction of soil chemical properties (organic matter (OM), pH, Ca, Mg, K, Na, total acidity, cation exchange capacity (CEC)) on 688 Korean soil samples using the visible-near infrared reflectance (VIS-NIR) spectroscopy. Reflectance from the visible to near-infrared spectrum (350 to 2500 nm) was acquired using the ASD Field Spec Pro. A total of 688 soil samples from 168 soil profiles were collected from 2009 to 2011. The spectra were resampled to 10 nm spacing and converted to the 1st derivative of absorbance (log (1/R)), which was used for predicting soil chemical properties. Principal components analysis (PCA), partial least squares regression (PLSR) and regression rules model (Cubist) were applied to predict soil chemical properties. The regression rules model (Cubist) showed the best results among these, with lower error on the calibration data. For quantitatively determining OM, total acidity, CEC, a VIS-NIR spectroscopy could be used as a routine method if the estimation quality is more improved.

Determination of total iodide in seawater by gas chromatography-mass spectrometry (Gas chromatography-mass spectrometry를 이용한 해수 중 총 요오드 정량분석)

  • Shin, Ueon-Sang
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.445-450
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    • 2002
  • A sensitive gas chromatographic method has been established for the determination of total iodide in seawater as their volatile organic derivative. The method is based on the formation of 4-iodo-2,6-dimethylphenol with 2,6-dimethylphenol in matrix and a single-step extraction of the derivative with ethyl ether, which are then measured by gas chromatography-mass spectrometry (selected ion monitoring). Iodate in sea water was completely reduced to iodide with ascorbic acid and acetic acid. The detection limit was 0.1 ng/mL in seawater and the calibration curve showed good linearity with r=0.9997. The method was sensitive, reproducible and simple enough to permit the reliable routine analysis of total iodide in seawater. Total iodide in sea water was found about 30 ng/ml.

A Modified Methylation Method to Determine Fatty Acid Content by Gas Chromatography

  • Wirasnita, Riry;Hadibarata, Tony;Novelina, Yus Maria;Yusoff, Abdull Rahim Mohd;Yusop, Zulkifli
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3239-3242
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    • 2013
  • An improved rapid method for determination of the fatty acid composition using modified methylation procedure was compared with the AOAC reference procedure based on the methylation of fatty acid with the addition of BF3 catalyst before and while heating. The new method is useful for research and routine quality control and has a number of advantages over the reference procedure which are more rapid, simple and also reliable. Applicability of the modified methylation method was confirmed with three vegetable oil samples (palm oil, coconut oil and olive oil). Based on the validation method results, we obtained that a quite linear calibration curve of fatty acids was performed with $R^2$ in range of 0.9972-0.9994. The sensitivity of gas chromatography instrument was able to analyze the fatty acids up to a few ppm, the precision and accuracy were good enough with the %RSD between 1.5%-19.5% and the recovery of linolenic acid was 99.1% in the range of 80.0%-113.3%.

HPLC SEPARATION AND QUANTITATIVE DETERMINATION OF GINSENOSIDES FROM PANAX GINSENG, PANAX QUINQUEFOLIUM AND FROM GINSENG DRUG PREPARATIONS

  • Soldati F
    • Proceedings of the Ginseng society Conference
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    • 1980.09a
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    • pp.59-69
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    • 1980
  • A new HPLC-method for separation and quantitative determination of ginsenosides in Panax ginseng, Panax quinquefolium and in pharmaceutical drug preparations is elaborated. A reversed-phase-system with ${\mu}Bondapak\;C_{18}$ column (3.9 mm $I.D.{\times}30\;cm$) using acetonitrile-water (30:70) 2 ml/min and acetonitrile-water (18:82) 4 ml/min is suitable for the base-line separation of $Rb_1,\;Rb_2,\;Rc,\;Rd,\;Rf,\;Rg_2,\;respectively\;Re,\;Rg_1$ in 30 minutes. The ginsenosides are directly detected at 203 nm (without derivatization) with the LC-55 or LC-75 spectrophotometer (Perkin-Elmer) at $100\%$ transmission. Detection limit is 300 ng at a signal-to-noise ratio of 10:1. The ginsenosides-peak identification is carried out with HPTLC (high performance thin layer chromatography), with MIR-IR (multiple internal reflection-IR-spectros-copy) and with FD-MS (field desorption mass spectrometry). The calibration curve of each ginsenoside has a correlation coefficient very near to 1. Relative standard deviation for quantitative determinations depends upon the amount of ginsenosides and is approximately 1\%$ for ginsenoside contents of 1\%$. This method is adaptable for routine analysis in quality control laboratories.

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Simultaneous HPLC Analysis of Three Flavonoids in the Extracts of Artocarpus heterophyllus Heartwoods

  • Septama, Abdi Wira;Panichayupakaranant, Pharkphoom
    • Natural Product Sciences
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    • v.22 no.2
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    • pp.77-81
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    • 2016
  • A reversed-phase high-performance liquid chromatographic method is described for the simultaneous determination of three antibacterial flavonoids, artocarpanone, artocarpin, and cycloartocarpin in ethyl acetate extracts from Artocarpus heterophyllus heartwoods. Separation was achieved using a TSK-gel ODS-80Tm column ($5{\mu}m$, $4.6{\times}150mm$) at $25^{\circ}C$ with a gradient elution system of methanol and water as follows: 0-8 min, 60:40; 8-27 min, 80:20; 27-35 min, 60:40, v/v, at a flow rate of 1 mL/min, and a quantitative UV detection at 285 nm. The method was validated by measuring the key parameters, including specificity, linearity, sensitivity, accuracy, repeatability and reproducibility. A high degree of specificity and sensitivity was achieved. The calibration curves for all three flavonoids showed good linearity with a coefficient of determinations ($R^2$) of ${\geq}0.9995$. The recoveries of the method were from 98-104%, with good reproducibility and repeatability (RSD values of less than 2%) were also achieved. Ethyl acetate was the best solvent for extraction of these three flavonoids using the heat reflux conditions for 1 h. This optimized sample preparation and HPLC method can be practically used for a routine standardization process of the extracts from the A. heterophyllus heartwoods.

Analysis of Mono-, Di- and Tri-glycerides by high-performance liquid chromatography (HPLC) with evaporative light scattering detection (ELSD) (HPLC/ELSD에 의한 Mono-, Di- 및 Tri-glycerides류 분석)

  • Lee, Man-Ho;Park, Heai-Ku;Kim, In-Whan
    • Analytical Science and Technology
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    • v.19 no.3
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    • pp.189-193
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    • 2006
  • Chromatographic separation of glycerol monostearate, glycerol distearate and glycerol tristearate (GMS, GDS, and GTS) has been performed by normal phase HPLC method utilizing a Zorbax silica ($250{\times}4.6mm$, $5{\mu}m$) column and hexane-hexane, IPA and ethyl acetate mixtures as the eluent within 20 min. The observed reproducibility was less than 5% RSD, Suggesting that ELSD was an effective tool for detection of the glycerol stearates of low volatility without chromophore. The detection limits were in the concentration range of 0.3~2 mg/L, and the calibration curves (the log-log plots) were linear in the range of 4~1000 mg/L (with the slopes of 1.06~1.32). The application of the analytical procedure without pretreatment demonstrated that the proposed chromatographic method would be practical for a routine analysis of commercial products.

Development of an analytical method for the quantification of oleanonic acid from mastic gum using HPLC/PDA

  • Hak-Dong Lee;Chang-Dae Lee;So Yeon Choi;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • v.66
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    • pp.67-72
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    • 2023
  • A simple and accurate method was developed for the quantitative analysis of oleanonic acid (OA) from mastic gum. The analysis was carried out using reverse-phase high-performance liquid chromatography combined with a photodiode array detector (HPLC/PDA). Our optimized method was validated by measuring various parameters, using an INNO C18 column fitted with a gradient elution system. The results revealed limits of detection and quantification of 0.34 and 1.042 ㎍/mL, respectively. The OA calibration curve exhibited excellent linearity over the concentration range of 0.0625 to 2.0 mg/mL, with r2 =0.9996. Accuracy tests revealed a high recovery rate of 99.44-103.66%, with precision values below 0.15%. These results suggest that the present analytical method can identify and quantify OA in mastic gum with high precision. The HPLC approach developed in this study might be applied to routine analyses and large-scale extraction procedures for OA content quantification.

THE EFFECT OF THE REPEATABILITY FILE IN THE NIRS EATTY ACIDS ANALYSIS OF ANIMAL EATS

  • Perez Marin, M.D.;De Pedro, E.;Garcia Olmo, J.;Garrido Varo, A.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.4107-4107
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    • 2001
  • Previous works have shown the viability of NIRS technology for the prediction of fatty acids in Iberian pig fat, but although the resulting equations showed high precision, in the predictions of new samples important fluctuations were detected, greater with the time passed from calibration development to NIRS analysis. This fact makes the use of NIRS calibrations in routine analysis difficult. Moreover, this problem only appears in products like fat, that show spectrums with very defined absorption peaks at some wavelengths. This circumstance causes a high sensibility to small changes of the instrument, which are not perceived with the normal checks. To avoid these inconveniences, the software WinISI 1.04 has a mathematic algorithm that consist of create a “Repeatability File”. This file is used during calibration development to minimize the variation sources that can affect the NIRS predictions. The objective of the current work is the evaluation of the use of a repeatability file in quantitative NIRS analysis of Iberian pig fat. A total of 188 samples of Iberian pig fat, produced by COVAP, were used. NIR data were recorded using a FOSS NIRSystems 6500 I spectrophotometer equipped with a spinning module. Samples were analysed by folded transmission, using two sample cells of 0.1mm pathlength and gold surface. High accuracy calibration equations were obtained, without and with repeatability file, to determine the content of six fatty acids: miristic (SECV$\sub$without/=0.07% r$^2$$\sub$without/=0.76 and SECV$\sub$with/=0.08% r$^2$$\sub$with/=0.65), Palmitic (SECV$\sub$without/=0.28 r$^2$$\sub$without/=0.97 and SECV$\sub$with/=0.24% r$^2$$\sub$with/=0.98), palmitoleic (SECV$\sub$without/=0.08 r$^2$$\sub$without/=0.94 and SECV$\sub$with/=0.09% r$^2$$\sub$with/=0.92), Stearic (SECV$\sub$without/=0.27 r$^2$$\sub$without/=0.97 and SECV$\sub$with/=0.29% r$^2$$\sub$with/=0.96), oleic (SECV$\sub$without/=0.20 r$^2$$\sub$without/=0.99 and SECV$\sub$with/=0.20% r$^2$$\sub$with/=0.99) and linoleic (SECV$\sub$without/=0.16 r$^2$$\sub$without/=0.98 and SECV$\sub$with/=0.16% r$^2$$\sub$with/=0.98). The use of a repeatability file like a tool to reduce the variation sources that can disturbed the prediction accuracy was very effective. Although in calibration results the differences are negligible, the effect caused by the repeatability file is appreciated mainly when are predicted new samples that are not in the calibration set and whose spectrum were recorded a long time after the equation development. In this case, bias values corresponding to fatty acids predictions were lower when the repeatability file was used: miristic (bias$\sub$without/=-0.05 and bias$\sub$with/=-0.04), Palmitic (bias$\sub$without/=-0.42 and bias$\sub$with/=-0.11), Palmitoleic (bias$\sub$without/=-0.03 and bias$\sub$with/=0.03), Stearic (bias$\sub$without/=0.47 and bias$\sub$with/=0.28), oleic (bias$\sub$without/=0.14 and bias$\sub$with/=-0.04) and linoleic (bias$\sub$without/=0.25 and bias$\sub$with/=-0.20).

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Quantitative Analysis of Effects for Quality Control on Medical Primary Class LCD Display Devices Based on AAPM TG18 Report (AAPM TG18에 의한 진단용 LCD 디스플레이 장치 정도관리 효과의 정량적 분석)

  • Jung Hai-Jo;Kim Hee-Joung
    • Progress in Medical Physics
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    • v.17 no.2
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    • pp.77-82
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    • 2006
  • The image display is an Important component of PACS and of medical digital imaging chain. Displayed image qualify is affected by the physical characteristics of display device, appropriate clinical settings and calibrations, and ambient lighting conditions. The performance of display systems is continuously degraded over time due to luminance deterioration and changes of clinical setting parameters. A routine QC is recommended because the performance of display systems is continuously degraded over time. Ten flat panel monochrome LCD display devices were included in the evaluation of the QC effect. The effect of QC on primary class LCD medical display devices for selected QC tests was evaluated by comparing the performances, luminance response, luminance dependencies, display resolution and display chromaticity in this study, of before and after the calibration procedures. The effects of the QC are significant to luminance response and luminance spatial dependencies test and the other side, are slight to the display resolution and display chromaticity test. A routine QC of display device is essential for the consistency of medical image display and presentation. The study of the QC effects of display devices will play an important role in practical QC procedures of display devices.

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Study for Residue Analysis of Pinoxaden in Agricultural Commodities

  • Kim, Ji Young;Yoon, Eun Kyung;Kim, Jong Soo;Seong, Nu Ri;Yun, Sang Soon;Jung, Yong Hyun;Oh, Jae Ho;Kim, Hyochin
    • Korean Journal of Environmental Agriculture
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    • v.38 no.4
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    • pp.321-331
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    • 2019
  • BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C18. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r2) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.