• Title/Summary/Keyword: % RSD

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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%.

Development of a Novel Sampling Technique for Natureal VOC Emissions

  • Kim, Jo-Chun
    • Journal of Korean Society for Atmospheric Environment
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    • v.17 no.E2
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    • pp.61-70
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    • 2001
  • In recent years there have been growing interests in the potential environmental effects of global climate change. Of specific interests is the role that climate change may play in altering natural volatile organic compound.(NVOC) emissions from trees and the subsequent impact of this perturbation on air quality and ozone formation. A novel vegetation enclosure chamber method was designed and constructed of Tedlar in order to estimate more accurate and precise NVOC emission rates of either small whole plants or the branches of large trees. The enclosure chamber was initially tested in the laboratory and also successfully evaluated in the field. Overall precision for this enclosure was estimated as RSD<10%(n=9). The overall errors associated with the enclosure method in a laboratory system might be relatively small (say<$\pm$15%); however, they might be rather large(say$\pm$40%) in a field-based system. Two consecutive samples were collected on each sampling day from the two pine species during the test period. Slash pine studies showed that the absolute percentage difference between the first and second samples varied from 0.33 to 29%. The percent differences between consecutive emission for loblolly pines varied from 0.74 to 24.2%.

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The Use of Crude Extract of Kohlrabi (Brassica oleracea gongylodes) as a Source of Peroxidase in the Spectrofluorimetric Determination of Thiamine

  • Amjadi, Mohammad;Manzoori, Jamshid L.;Orooji, Maghsood
    • Bulletin of the Korean Chemical Society
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    • v.28 no.2
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    • pp.246-250
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    • 2007
  • The crude extract of kohlrabi (Brassica oleracea gongylodes) was prepared as a rich source of peroxidase and its enzymatic and specific activities in the presence of cross-linked polyvinylpyrrolidone as a stabilizer were determined. This extract was used to catalyze the oxidation of thiamine in the presence of hydrogen peroxide to thiochrome at pH 8.0. Thiochrome shows strong fluorescence at 436 nm with excitation at 370 nm. Based on the obtained results, a sensitive and simple spectrofluorimetric method was developed for the determination of thiamine. In the optimum conditions, the calibration graph was linear from 2 × 10-7 to 1 × 10-4 mol L-1, with a detection limit of 6.2 × 10-8 mol L-1. The relative standard deviation (RSD) was 1.2% for 5 × 10-6 mol L-1 thiamine. The method was successfully applied to the determination of thiamine in vitamin B1 and vitamin B complex tablets and vitamin B complex syrup.

The Interaction of CO to the Co(salen) Complex in to PEDOT:PSS Film and Sensor Application

  • Memarzadeh, Raheleh;Panahi, Farhad;Javadpour, Sirus;Ali, Khalafi-Nezhad;Noh, Hui-Bog;Shim, Yoon-Bo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.4
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    • pp.1297-1302
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    • 2012
  • The interaction between carbon monoxide (CO) and a cobalt-salen complex (Co(salen)) was studied and applied to detect CO. The metal complex doped PEDOT:PSS film exhibited good sensitivity to CO and differentiate CO from other gases. The response of the composite to CO was reversible (RSD < 5%) change in resistance upon removal of CO gas from the test chamber. The effects of adding Co(salen) in the probe film on the response of the sensor were investigated using AFM, XPS, and FT-IR spectroscopy. The sensitivity of the sensor increased as the Co(salen) concentration enhanced as it increased from 0.0 to 1.5 wt. %, where the highest sensitivity ($%{\Delta}R/R_o$) of $-25.0{\pm}0.05%$ was achieved with 1.0 wt. % Co(salen). The sensor containing probe exhibited a linear response ($R^2$ = 0.983) in the range of 0.5 to 10.0% CO (v/v) $N_2$, and the detection limit was 1.74% CO (v/v) in $N_2$.

Homogeneous Enzyme-Linked Binding Assay Mediated by the Interaction of Avidin with Biotin: Mistletoe Lectin I Assay

  • Rhee Paeng, In-Suk;Lee, Eun-Ah;Kim, Hyun-Sook
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.115-118
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    • 2004
  • We have examined the feasibility of using the specific interaction between mistletoe lectin I (ML I) and ${\beta}$-Dgalactose instead of the anti-ML I antibody in developing a homogeneous type competitive binding assay for ML I. We also have examined the feasibility of adapting the biotin/avidin mediated homogeneous assay for this system. Alkaline phosphatase (AKP) was employed as a single substrate enzyme label. The dose-response curve shows a detection range of 1-25 ${\mu}$g/mL and a linear response with a correlation coefficient of 0.99. To demonstrate the analytical utility of this method, 10 ${\mu}$g/mL of ML I was spiked into distilled water. The results show that the mean recovery was 10.03 ${\mu}$g/mL with an SD of 0.18. The difference between the spiked value and the mean recovery was 0.03 ${\mu}$g/mL, with a relative error of 0.3 and 1.6 % of RSD.

Removal of Aluminum from Water Samples by Sorption onto Powdered Activated Carbon Prepared from Olive Stones

  • Ghazy, S.E.;El-Morsy, S.M.
    • Carbon letters
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    • v.8 no.3
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    • pp.191-198
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    • 2007
  • Recent studies have revealed the poisonous nature of aluminum(III) species to aquatic and terrestrial organisms. Therefore, this investigation aims to develop batch adsorption experiments in the laboratory, aiming to the removal of aluminum(III) from aqueous solutions onto powdered activated carbon (PAC). The latter (which is an effective and inexpensive sorbent) was prepared from olive stones generated as plant wastes and modified with an aqueous modifying oxidizing agent, viz. $HNO_3$. The main parameters (i.e. initial solution pH, sorbent and $Al^{3+}$ ions concentrations, stirring times and temperature) influencing the sorption process were examined. The results obtained revealed that the sorption of $Al^{3+}$ ions onto PAC is endothermic in nature and follows first-order kinetics. The adsorption data were well described by the Langmuir, Freundlich and Dubinin-Radushkevich (D-R) adsorption models over the concentration range studied. Under the optimum experimental conditions employed, the removal of ca. 100% $Al^{3+}$ ions in the concentration range $1.35-2.75\;mg{\cdot}l^{-1}$ was attained. Moreover, the procedure was successfully applied to the recovery of aluminum spiked to some environmental water samples with an RSD (%), does not exceed 1.22%.

Determination of DBCP and n-Butylbenzene using SPME with GC-MS (SPME-GC-MS를 이용한 DBCP 및 n-Butylbenzene의 분석)

  • Park, Hyun-Mee;Kim, Young-Man;Lee, Dai-Woon;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.14 no.6
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    • pp.471-475
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    • 2001
  • Solid phase microextraction(SPME) with $85{\mu}m$-polyacrylate (PA) and $100{\mu}m$-polydimethylsiloxane(PDMS) fibers, coupled to gas chromatography-mass spectrometry was used to determine 1,2-dibromo-3-chloropropane(DBCP) and n-butylbenzene in water. The conditions affecting the SPME process(i.e, extraction time, injection length, injection temperature, desorption time and temperature) were optimized. The linearity of the calibration curve (correlation coefficient, R) was over 0.99 and the limits of detection of the method were between 1.5 and $10.8{\mu}g/L$. Repeatability of the method was between 10.4 and 14.4 %.

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$H_2O_2$ Detection Property of Glucose Sensor using Self Assembled Viologen Modified Electrode as Mediator (Viologen 유도체를 전하전달체로 이용한 Glucose 센서의 $H_2O_2$ 검출 특성)

  • Lee, Dong-Yun;Choi, Won-Suk;Park, Sang-Hyun;Kwon, Young-Soo
    • Proceedings of the KIEE Conference
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    • 2007.11a
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    • pp.86-87
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    • 2007
  • An amperometric glucose biosensor has been developed using viologen derivatives as electron mediator of glucose oxidase (GOD) at Au electrode. Highly stable self assembled monolayer (SAM) of thiol-based viologen is immobilized onto the Au electrode followed byGOD is immobilized onto the viologen modified electrode. This biosensor response to glucose was evaluated amperometrically in the potential of -300 mV. Upon immobilization of glucose oxidase onto the viologen modified-electrode, the biosensor showed rapid response towards glucose. Experimental conditions influencing the biosensor performance such as, pH, potential were optimized and assessed. This biosensor offered an excellent electrochemical response for glucose concentration below ${\mu}mol$ level with high sensitivity and selectivity and short response time. The levels of the RSD's (< 5 %) for the entire analyses reflected the highly reproducible sensor performance. Using the optimized a linear relationship between current and glucose concentration was obtained up to $4.5{\times}10^{-4}$ M. In addition, this biosensor showed well reproducibility and stability.

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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.

Simultaneous Analysis of Liquiritin and Glycyrrhizin in Sagunja-tang by HPLC-PDA (HPLC-PDA에 의한 사군자탕 중 Liquiritin과 Glycyrrhizin의 동시분석)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.42 no.3
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    • pp.240-245
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    • 2011
  • A high-performance liquid chromatography (HPLC) method was developed for quantitative analysis of liquiritin and glycyrrhizin in Sagunja-tang (SGT, Sijunzi-tang in Chinese), a traditional Korean medicine. HPLC analysis was performed using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 254 nm and 280 nm for quantification of the two components in SGT. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Calibration curves were acquired with $r^2$ values > 0.9998, and the relative standard deviations (RSDs, %) for intra- and inter-day precision were not exceed 4.0%. The recovery of each component was in the range of 91.85 - 108.62%, with a RSD less than 4.0%. The contents of the two components in SGT were 7.94 - 13.83 mg/g.