• Title/Summary/Keyword: eluent

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Determination of blood concentration of higenamine by high pressure liquid chromatography

  • Park, Sun-Oak;Hong, Chang-Yee;Paik, Seung-Whan;YunChoi, Hye-Sook
    • Archives of Pharmacal Research
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    • v.10 no.1
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    • pp.60-66
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    • 1987
  • A procedure utilizing high pressure liquid chroatography coupled with UV detection is described for the determination of blood concentration of higenamine. Deproteinized serum was pretreated with$C_{18}$(Sep-pak $C_{18}$ cartridge) and the 70% EtOH eluent was applied onto a reversed-phase column ($\mu$ Bondapak $C_{18}]$) with a 15% acetonitrile in 0.05 N $NaH_2$$PO_4$-trichloroacetic acid mixed buffer (pH 2.8) as a mobile phase. With the UV detection at 232 nm, the retention times of higenamine and 1, 2, 3, 4-tetrahydropapaveroline, an internal standard, were 5.2 min and 3.9 min respectively. The blood concentration of higenamine was meausred at regular intervals after i. v. injection of higenamine to rabbit. A drastic decrease in higenamine concentration to 30% of the maximum value obtained immediately after the injection, was observed during the first 1-2 min period and thereafter the rate of decrease was slowed down. The analytical result seemed to coincide with the pharmacological effect of higenamine exerting the maximum chronotropic and hypotensive effect at the completion of the injections which were progressively recovered.

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Studies on Simultaneous Analysis of Organophosphorus Pesticide Residues in Crops by Gas-Liquid Chromatography (I) Extraction and Cleanup (기체-액체 크로마토그래피에 의한 농작물 중 유기인제 잔류 농약의 동시 분석에 관한 연구 (제 1 보). 용매추출 및 방해성분의 분리 제거)

  • Taek-Jae Kim;Yun-Woo Eo;Young Sang Kim
    • Journal of the Korean Chemical Society
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    • v.30 no.5
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    • pp.465-474
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    • 1986
  • The solvent extraction and cleanup processes for the simultaneous gas-liquid chromatographic determination of 11 kinds of organophosphorous pesticide residues in crops were investigated. The extracts dissolved with acetone were partitioned with petroleum ether after adding saturated NaCl solution. Evaporated the partitioning solvent, the residue was dissolved in methylene chloride and eluted through mixed adsorbent (1 : 2 : 4 of activated carbon, magnesia and diatomaceous earth) with methylene chloride as an eluent. The pesticides recovered were 82∼105% and the impurities were effectively removed.

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Analysis of Cationic Surfactants in Cosmetics By Reverse phase Ion-Pair Chromatigraphy with Suressed Conductivity Detector and UV Detector

  • Jong-Keun Choi;Jae
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.23 no.3
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    • pp.161-167
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    • 1997
  • Determination of several cationic surfactants in cosmetics has been investigated. Reverse phase ion pair chromatography was used to identify and quantitate cationic surfactants. Cationic surfactants analyzed in this experiment were cetylpyridium chloride, stearyltrimetylammonium chloride, bezalkonium chloride, benzyldicethylcetylammonium chloride, and bihenyltrimethyl ammonium chloride. The separation was achieved on a reverse phase coumn with 10mM HCl-acetonitrile eluent. In this condition, the most of cationic surfactants with exception of CPC and CTAC respectively with suppressed conductivity detector and UV detector connected in series. The calibration curves obtained by plotting the peak areas of the cationic surfactants were linear at levels ranging from 0.005 to 0.1% correlation coefficient, r=0.9988. The detection limits were 1 to 5ppm in sample solution. The average recoveries of cationic surfactants added to hair treatment cream and hair rinse in three to five experiments were 96.7 105.2% and relative standard deviations were 1.1-3.8%. The case that there were CPC and CTAC in same solution was also tested. CPC and CTAC which couldn't be separated on reverse phase column were quantitated with suppressed conductivity detector and UV detector connected in series. Recovery of CPC and CTAC were 101.6 and 89.2% respectively. The proposed method was applied to the determination of cationic surfactants in commercial hair treatment cream.

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Elution Behavior of Copper(II) and Iron(II) Ions by Phenol Sulfonic Acid on Chelating Resin (킬레이트 수지에서 Phenol Sulfonic Acid에 의한 구리(Ⅱ)와 철(Ⅱ) 이온의 용리현상)

  • Cha, Ki Won;Hong, Jang Wook;Choi, Bae Du
    • Journal of the Korean Chemical Society
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    • v.42 no.3
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    • pp.292-296
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    • 1998
  • The elution behavior of copper(Ⅱ) and iron(Ⅱ) ions by phenol sulfonic acid(PSA) as an eluent on chelating resin, Amberlite IRC-718 have been investigated. When copper(Ⅱ) and iron(Ⅱ) solutions were adsorbed on the resin and eluted with various concentration of PSA, two peaks of each ion were appeared in the elution curve. These two peak areas were changed according to the PSA concentration. Using these phenomena, the stability constants of complex formation between the two ions and PSA were calculated. The values are 7.0 for copper(II) and $4.5{\times}10^4$ for iron(II), respectively.

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Preconcentration and Determination of Fe(III) from Water and Food Samples by Newly Synthesized Chelating Reagent Impregnated Amberlite XAD-16 Resin

  • Tokahoglu, Serife;Ergun, Hasan;Cukurovah, Alaaddin
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1976-1980
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    • 2010
  • A simple and reliable method has been developed to selectively separate and concentrate trace amounts of Fe(III) ions from water and food samples by using flame atomic absorption spectrometry. A new reagent, 5-hydroxy-4-ethyl-5,6-di-pyridin-2-yl-4,5-dihydro-2H-[1,2,4] triazine-3-thione, was synthesized and characterized by using FT-IR spectroscopy and elemental analysis. Effects of pH, concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of Fe(III) were investigated. The optimum pH was found to be 5. Eluent for quantitative elution was 10 mL of 2 M HCl. The preconcentration factor of the method, detection limit (3s/b, ${\mu}gL^{-1}$) and relative standard deviation values were found to be 25, 4.59 and 1%, respectively. In order to verify the accuracy of the method, two certified reference materials (TMDA 54.4 lake water and SRM 1568a rice flour) were analyzed. The results obtained were in good agreement with the certified values. The method was successfully applied to the determination of Fe(III) ions in water and food samples.

Separation and Elution Behavior of Cations Based on Distribution Coefficients (분포계수를 토대로한 양이온의 용리현상 및 분리)

  • Dong Won Kim;Song Reck Park;Yong Whan Kang;Nam Kee Rhee
    • Journal of the Korean Chemical Society
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    • v.24 no.5
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    • pp.361-370
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    • 1980
  • Distribution coefficients of various elements with the strong acidic caion-exchanger, Dowex 50W-x8, 100∼200 mesh were investigated in various concentrations of succinic, hydrochloic acid and it's mixture. Based on these distribution coefficients,the experimental condition for their quantitative separation of those elements is established in 0.9 M hydrochloric acid as eluent, several examples of successful separations are described and the dependence of distribution coefficients on ionic radius is also discussed.

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Sorption and Separation of Thiocyanate Gold and Silver Complexes and Determination of Gold by Diffuse Reflectance Spectroscopy

  • Danilenko, N.V.;Kononova, O.N.;Kachin, S.V.;Kholmogorov, A.G.;Dmitrieva, Zh.V.;Plotnikova, E.A.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.7
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    • pp.1019-1024
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    • 2004
  • The present paper is focused on simultaneous sorption concentration of gold (III) and silver (I) from thiocyanate solutions using high-selective anion exchanger AN-25 and subsequent separation of these ions at various concentrations of thiocarbamide (eluent). As a result, silver (I) ions are completely eluted from AN-25 and gold (III) ions remain in the resin phase and can be determined directly in the solid phase by diffuse reflection spectroscopy. It is proposed to use the sorption-spectroscopic method for Au(III) determination in aqueous solutions. The calibration curve is linear in the concentration range of 1-19 mg/L (sample volume is 10.0 mL) and the detection limit is 0.05 ${\mu}g/mL$. The presence of Cu(II), Co(II), Fe(II) do not hinder this determination. Au(III) was determined in industrial solutions.

Determination of nickel and cadmium in fish, canned tuna, black tea, and human urine samples after extraction by a novel quinoline thioacetamide functionalized magnetite/graphene oxide nanocomposite

  • Naghibzadeh, Leila;Manoochehri, Mahboobeh
    • Carbon letters
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    • v.26
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    • pp.43-50
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    • 2018
  • In this research, a novel and efficient quinoline thioacetamide functionalized magnetic graphene oxide composite ($GO@Fe_3O_4@QTA$) was synthesized and utilized for dispersive magnetic solid phase preconcentration of Cd(II) and Ni(II) ions in urine and various food samples. A number of diverse methods were employed for characterization of the new nanosorbent. The design of experiments approach and response surface methodology were applied to monitor and find the parameters that affect the extraction performance. After sorption and elution steps, the concentrations of target analytes were measured by employing FAAS. The highest extraction performance was achieved under the following experimental conditions: pH, 5.8; sorption time, 6.0 min; $GO@Fe_3O_4@QTA$ amount, 17 mg; 2.4 mL $1.1mol\;L^{-l}$ $HNO_3$ solution as the eluent and elution time, 13.0 min. The detection limit is 0.02 and $0.2ng\;mL^{-1}$ for Cd(II), and Ni(II) ions, respectively. The accuracy of the new method was investigated by analyzing two certified reference materials (sea food mix, Seronorm LOT NO 2525 urine powder). The interfering study revealed that there are no interferences from commonly occurring ions on the extractability of target ions. Finally, the new method was satisfactorily employed for rapid extraction and determination of target ions in urine and various food samples.

Measurement of optical purity for commercial naproxen by chiral HPLC (키랄 크로마토그래피에 의한 시판되는 나프록센의 광학순도 측정)

  • Yu, Jeong-Jae;Lee, Won-Doo;Ryoo, Jae-Jeong
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.360-367
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    • 2011
  • Optical purities of 10 commercialized naproxens prepared from eight Korean drug companies were examined by an optimized chiral HPLC condition. The Chiralcel OD-H column and ChiralHyun-LE(S)-1 column were used as chiral stationary phases and the mixed eluent of hexane/isopropanol/acetic acid as 100:2.85:0.1 was used as a mobile phase for effective enantioseparation. Optical purity values of most samples were higher than 97 percents, only one of them was about 95 percents. The average relative standard deviation of them appeared very small (0.034%).

Sterin C, a New Antioxidant from the Mycelial Culture of the Mushroom Stereum hirsutum

  • Yoo, Nam-Hee;Yoo, Ick-Dong;Kim, Jin-Woo;Yun, Bong-Sik;Ryoo, In-Ja;Yoon, Eui-Soo;Chinh, Nguyen Thi;Kim, Jong-Pyung
    • Journal of Applied Biological Chemistry
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    • v.48 no.1
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    • pp.38-41
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    • 2005
  • Structurally new antioxidative metabolite was isolated from mycelial culture of mushroom Stereum hirsutum. Culture broth was subjected to Diaion HP-20 column chromatography, and 70% aqueous MeOH eluent was extracted with EtOAc. EtOAc extract was purified through silica gel and Sephadex LH-20 column chromatographies, and reversed phase $C_{18}$ HPLC. Compound was revealed to be new dihydroxylated derivative of sterin B with molecular formula of $C_{12}H_{16}O_5$(MW 240) by MS and various NMR spectral data analyses, and designated as sterin C. Sterin C showed superoxide radical-scavenging activity with $EC_{50}$ value of 0.31 mM.