• Title/Summary/Keyword: Chemical Determination

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Determination of Selenium in Foods by HG-AAS (HG-AAS에 의한 식품 중의 셀렌의 정량에 대한 연구)

  • Ki-Won Cha;Sang-Ho Park;Jae-Sung Choi
    • Journal of the Korean Chemical Society
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    • v.38 no.12
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    • pp.891-897
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    • 1994
  • A method has been investigated for the determination of Selenium in Ginseng radix, Ganoderma Lucidum and Garlic using hydride generation atomic absorption spectrometry (HG-AAS). The effects of several acids and sodium tetrahydroborate concentration and their flow rate on the determination of Selenium for the hydride generation were investigated. The method of sample decomposition was also investigated using various mineral acids, such as nitric, perchloric and sulfuric acid in the closed system and foreign ion effects were studied. In the optimum conditions, we obtained calibration curve in the range 0-40 ppb. The analytical data of Garlic, Ganoderma Lucidum and Ginseng radix are 289, 296, 198 ppb, respectively.

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Determination of Coccidiostats (Amprolium and Decoquinate) in Cattle and Chicken's Muscle using High Performance Liquid Chromatography

  • Kim, Byung-Ju;Ham, Hyun-Sun;Lee, Jin-Joo;Cheong, Nam-Yong;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.559-563
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    • 2012
  • An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

Synthesis of a New α-Dioxime Derivative and Its Application for Selective Homogeneous Liquid-Liquid Extraction of Cu(II) into a Microdroplet Followed by Direct GFAAS Determination

  • Ghiasvand, A. R.;Shadabi, S.;Kakanejadifard, A.;Khajehkoolaki, A.
    • Bulletin of the Korean Chemical Society
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    • v.26 no.5
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    • pp.781-785
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    • 2005
  • A fast and reliable method for the selective separation and preconcentration of $Cu^{2+}$ ions using homogeneous liquid-liquid extraction was developed. A new $\alpha$-dioxime derivative (2H-1,4-benzothioazine-2,3(4H)dionedioxime, Dioxime I) was synthesized and investigated as a suitable selective complexing ligand for $Cu^{2+}$ ions. Zonyl FSA (FSA) was applied as a phase-separator agent under the slightly acidic pH conditions. Under the optimal experimental conditions ([FSA] = 3.2% w/v, [THF] = 19.5% v/v, [Dioxime I] = 1.9 ${\times}\;10^{-3}$ M, and pH = 4.7), 10 ${\mu}g\;of\;Cu^{2+}$ in 5.2 mL aqueous phase could be extracted quantitatively into 80 $\mu$L of the sedimented phase. The maximum concentration factor was 65-fold. The limit of detection of the proposed method was 0.005 ng $mL^{-1}$. The reproducibility of the proposed method, on the 10 replicate measurements, was 1.3%. The influence of the pH, type and volume of the water-miscible organic solvent, concentration of FSA, concentration of the complexing ligand and the effect of different diverse ions on the extraction and determination of $Cu^{2+}$ ions were investigated. The proposed method was applied to the extraction and determination of $Cu^{2+}$ ion in different synthetic and natural water samples.

Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.545-548
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    • 2004
  • A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with $C_{18}$ membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with $C_{18}$ membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was $1.32{\times}10^5L\;mol^{-1}cm^{- 1}$ at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 ${\mu}$g/mL. This method was applied to the determination of nickel in water and biological samples with good results.

Study on the Solid Phase Extraction of Hg(II)-SBDTR Chelate with C18 Disks and Its Application to the Determination of Mercury in Tobacco and Tobacco Additive

  • Yang, Guan-Gyu;Xia, Zhen-Yuang;Wu, Yu-Ping;Sun, Han-Dong;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.549-552
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    • 2004
  • A sensitive, selective and rapid method has been developed for the determination of mercury based on the rapid reaction of mercury(II) with p-sulfobenzylidenethiorhodanine (SBDTR) and the solid phase extraction of the colored chelate with $C_{18}$ disks. In the presence of pH 3.5 sodium acetate-acetic acid buffer solution and Emulsifier-OP medium, SBDTR reacts with mercury(II) to form a red chelate of a molar ratio 1 : 2 (mercury to SBDTR). This chelate was prconcentrated by solid phase extraction with $C_{18}$ disks. An enrichment factor of 50 was achieved. The molar absorptivity of the chelate is $1.28{\times}10^5 L{\cdot}mol^{-1}{\cdot}cm^{-1}$ at 545 nm in measured solution. Beer's law is obeyed in the range of 0.01-3 ${\mu}$g/mL. The relative standard deviation for eleven replicates sample of 0.01 ${\mu}$g/mL is 1.65%. This method was applied to the determination of mercury in tobacco and tobacco additive with good results.

Preconcentration of Copper(II) Using Mesoporous Organo-Silicas and Determination by Flame Atomic Absorption Spectrometry (메조다공성 유기-실리카를 이용한 구리(II)의 예비농축과 불꽃원자 흡수분광법으로의 정량)

  • Moghimi, Ali
    • Journal of the Korean Chemical Society
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    • v.52 no.2
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    • pp.155-163
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    • 2008
  • .A simple and reproducible method for the rapid extraction and determination of trace amounts of copper(II) ions using mesoporous organo-silicas mesoporous silica and atomic absorption spectrometry is presented. Common coexisting ions did not interfere with the separation and determination. The preconcentration factor was 100 (1 ml elution volume) for a 100 ml sample volume. The limit of detection of the proposed method is 1.0 ng ml-1. The maximum sorption capacity of sorbent under optimum conditions has been found to be 5mg of copper per gram of sorbent. The relative standard deviation under optimum conditions was 2.8% (n=10). Accuracy and application of the method was estimated by using test samples of natural and synthetic water spiked with different amounts of copper(II) ion.

A Comparison of Analytical Methods for the Content and Purity of Cefradine

  • Hyun, Myung-Ho;Jeong, Euh-Duck;Shin, Min-Seob;Jin, Jong-Sung
    • Bulletin of the Korean Chemical Society
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    • v.29 no.6
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    • pp.1185-1189
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    • 2008
  • Two HPLC methods such as cefadroxil and cefalexin methods were compared in their performance for the quantitative analysis of the content and purity of $\beta$ -lactamic antibiotic, cefradine, for six bulk drug samples. Between the two methods, the cefadroxil method prescribed by the European Pharmacopoeia (EP) for the determination of impurities in cefradoxil was superior to the cefalexin method prescribed by the EP and by the United States Pharmacopeia (USP) for the determination of cefalexin impurity in cefradine in terms of the greater stability of the chromatogram baselines and the higher precision, i.e., the lower % relative standard deviation (RSD). Based on the comparison of the two HPLC methods, the cefadroxil method was recommended to replace the TLC method, which has been prescribed by the EP as the official method for determination of extraneous impurities in cefradine.

Determination of Boron Isotopic Ratio by Using an Alpha Track Technique

  • Park, Yong-Joon;Pyo, Hyung-Yeal;Song, Kyu-Seok;Song, Byoung-Chul;Jee, Kwang-Yong;Kim, Won-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.10
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    • pp.1609-1612
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    • 2006
  • The determination of the boron isotopic ratio in solutions was achieved by means of a solid state track detector by using an alpha track. The neutron flux was optimized by using a Cd-foil to find the optimum conditions for counting the number of alpha tracks on the selected solid detector caused by the (n, $\alpha$) nuclear reaction of boron. The home-made multi-dot detector plate was utilized in this study to increase the reproducibility of the measurement by uniformly drying the boron solution within the marked circle area on the detector plate. The experimental results of this study verified that the $^{11}B/^{10}B $ isotopic ratio can be measured by observing the number of alpha tracks for different concentrated standard solutions with various isotopic compositions. This technique was applied to the determination of $^{10}B$ enrichment factor in a biological sample for a boron neutron capture therapy.

Study on Solid Phase Extraction and Spectrophotometric Determination of Vanadium with 2-(2-Quinolylazo)-5-Diethylaminophenol

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.263-266
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    • 2004
  • A sensitive, selective and rapid method has been developed for the determination ${\mu}$g/L level of vanadium ion based on the rapid reaction of vanadium(V) with 2-(2-quinolylazo)-5-diethylaminophenol (QADEAP) and the solid phase extraction of the colored chelate with $C_{18}$ cartridge. The QADEAP reacts with V(V) in the presence of citric acid-sodium hydroxide buffer solution (pH = 3.5) and cetyl trimethylammonium bromide (CTMAB) medium to form a violet chelate of a molar ratio 1 : 2 (V(V) to QADEAP). This chelate was enriched by solid phase extraction with $C_{18}$cartridge and the enrichment factor of 50 was obtained by elution of the chelates from the cartridge with ethanol. The molar absorptivity of the chelate is $1.28 {\times}10^5L\;mol^{-1}cm^{-1}$ at 590 nm in the measured solution. Beer's law is obeyed in the range of 0.01-0.6 ${\mu}$g/mL. The detection limit is 0.04 ${\mu}$g/L in the original samples. This method was applied to the determination of vanadium(V) in water and biological samples with good results.

Selective Determination of Serotonin on Poly(3,4-ethylenedioxy pyrrole)-single-walled Carbon Nanotube-Modified Glassy Carbon Electrodes

  • Kim, Seul-Ki;Bae, Si-Ra;Ahmed, Mohammad Shamsuddin;You, Jung-Min;Jeon, Seung-Won
    • Bulletin of the Korean Chemical Society
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    • v.32 no.4
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    • pp.1215-1220
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    • 2011
  • An electrochemically-modified electrode [P(EDOP-SWNTs)/GCE] was prepared by electropolymerization of 3,4-ethylenedioxy pyrrole (EDOP) single-walled carbon nanotubes (SWNTs) on the surface of a glassy carbon electrode (GCE) and characterized by SEM, CV, and DPV. This modified electrode was employed as an electrochemical biosensor for the selective determination of serotonin concentrations at pH 7.4 and exhibited a typical enhanced effect on the current response of serotonin with a lower oxidation overpotential. The linear response was in the range of $1.0{\times}10^{-7}$ to $1.0{\times}10^{-5}$ M, with a correlation coefficient of 0.998 on the anodic current. The lower detection limit was calculated as 5.0 nM. Due to the relatively low currents and difference of potentials in the electrochemical responses of uric acid (UA), ascorbic acid (AA), and dopamine (DA), the modified electrode was a useful and effective sensing device for the selective and sensitive serotonin determination in the presence of UA, AA, and DA.