• Journal of Korean Society of Environmental Engineers
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• v.35 no.7
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• pp.485-494
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• 2013

An efficient extraction method was developed for the analysis of 16 perfluorinated compounds (PFCs) in fish samples. We compared the recoveries from the Ion-Pairing Extraction (IPE), Liquid-Liquid Extraction (LLE), Solid-Phase Extraction (SPE), IPE + SPE method with varying the injection time of the internal standard. As a result, IPE method with the internal standard before extraction was evaluated as the most effective pretreatment method. The RPM (Revolution Per Munite) and pH in IPE-before method were additionally adjusted and the more efficient pretreatment method was established. The total 33 fish samples including liver and gut samples were collected from Korean markets and analyzed PFCs with developed pretreatment method of this study. Total 16 PFC levels in fish samples ranged from ND to 1.67 ng/g with 100% detection frequency. The average PFCs concentrations of muscle, liver and gut samples from fish were compared and showed the following trend: liver (17.8 ng/g) > gut (13.3 ng/g) > muscle (1.67 ng/g). The PFC levels in fish samples were similar or lower than other available previous results of foreign studies.

• Analytical Science and Technology
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• v.6 no.3
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• pp.289-296
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• 1993

The formation of Mo(VI)-alizarin red S chelate ion and its extraction into an organic solvent by ion-pairing were studied for the separative determination of trace Mo(VI) in natural water samples. Natural water 100mL was sampled in 250mL separatory funnel. After Mo(VI)-ARS chelate ion was formed by adding 0.01M alizarin red S solution 0.5mL to the water sample of pH 4.0, 0.2% aliquat-336 chloroform solution 10mL was added and the solution was vigorously shaked for about 30 seconds to from the ion-pair between Mo(VI)-ARS and aliquat-336, completely. The solution was stood for about 90 minutes. And the organic phase was taken for the absorbance measurement of the ion-pair at 520 nm. The content of Mo(VI) in sample was obtained from the standard calibration curve. Several extraction conditions such as pH, adding amounts of alizarin red S and aliquat-336, and shaking and standing times were optimized. This procedure was applied to the analysis of river and tap waters. It could be confirmed from the recoveries of over 99% in samples spiked with a given amount of Mo(VI) that this method was quantitiative in the determination of trace Mo(VI) in a natural water.

• Analytical Science and Technology
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• v.7 no.3
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• pp.413-419
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• 1994

The determination of the neuromuscular blocking agents vecuronium bromide(VeBr) in biological fluids has been investigated. The method depends on the formation of insoluble red complex between vecuronium bromide and rose bengal in aqueous layer. The amount of vecuronium bromide was calculated from that of extracted rose bengal which was determined by spectrofluorimetry or HPLC/fluorescence detection method. It was possible to analyze VeBr in the range of $2{\sim}32{\mu}g/ml$(r=0.998 for water soln., 0.999 for urine, 0.996 for plasma). This method was applied to the analysis of VeBr in biological fluids, urine and plasma.

• Analytical Science and Technology
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• v.6 no.3
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• pp.329-334
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• 1993

The formation of Mo(VI)-alizarin red S chelate ion its extraction into an organic solvent by ion-pairing for the separarive determination of trace Mo(VI) in natural water was applied in seawater samples. Removed Fe(III) and Zn(II), and Cu(II) by precipitating with anthranilic acid at pH 4.0 and 2.0, seawater 100mL was sampled in 250mL separatory funnel. After Mo(VI)-ARS chelate ion was formed by adding 0.01M alizarin red S solution 1.0mL to the water sample of pH 4.6, 0.6% aliquat-336 chloroform solution 10mL was added and the solution was vigorously shaked for about 30 seconds to form the ion-pair between Mo(VI)-ARS and aliquat-336 perfectly. The solution was stood for about 30 minutes. And the organic phase was taken for the absorbance measurement of the ion-pair at 520nm. The content of Mo(VI) was obtained from the standard calibration curve. Several extraction conditions such as pH, adding amounts of alizarin red S and aliquat-336, and shaking and standing times were optimized and the interferences and release of concomitant ions was also studied. This procedure was applied to the analysis of Eastern and Yellow seawaters. It could be confirmed from the recoveries of over 85% in samples spiked with a given amount of Mo(VI) that this method was also quantitative in the determination of trace Mo(VI) in a seawater.

• Analytical Science and Technology
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• v.7 no.3
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• pp.261-269
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• 1994

The iodide formed stoichiometrically for sulfide by its oxidation with iodate was extracted as an ion-pair with methylene green into 1,2-dichloroethane and the extract was measured spectrophotometrically at 656nm for the determination of sulfide. Hydrogen sulfide separated from the sample matrix was introduced into a solution containing pH 3.5 acetate buffer and iodate, in which the hydrogen sulfide was completely converted into iodide. A linear calibration graph was obtained over the range $3{\times}10^{-7}{\sim}1.2{\times}10^{-5}M$ sulfide($0.0096{\sim}0.384{\mu}g$ of $S^{2-}/ml$) and the detection limit was $0.0032{\mu}g/ml$. The apparent molar absorptivity and a correlation coefficient(r) were $6.7{\times}10^4L\;mole^{-1}\;cm^{-1}$ and 0.999, respectively. When applied to the stream water samples, the proposed method gave a relative standard deviation of 1.59% at $5{\times}10^{-6}M$ sulfide level.

• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.423-432
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• 1986

Atomic absorption spectrophotometric (AAS) determination of hexavalent chromium [Cr(VI)] in a waste water was studied. Cr(VI) was extracted with p-xylene from the wastewater, in the way of ion pair formation with anion exchanger aliquat-336(tri-caprylmethyl ammonium chloride). 100ml waste water, after organic materials were extracted out with toluene, was acidified with conc. HCl adjusting the medium to pH 0.5 and 20ml of p-xylene containing 0.01M aliguat-336 was used to extract Cr(VI) from the acidified solution. The absorbance of chromium was measured with air-acetylene flame at 357.9nm. Standard addition method was used in the determining concentration of Cr(VI) extracted. No interference has been found in the extraction of Cr(VI) by the Al(III), Fe(III) and Cr(III) ion presented. However, Fe(II) decreased the absorbance of Cr(VI), due to the fact Fe(II) reduces Cr(VI) to Cr(III). The contained organic material was removed prior to extracting process, since it may reduced the absorbance of Cr(VI). The recovery of added Cr(VI) was over 96%, which seems to be promising and the relative standard deviation was 3.95%

• Analytical Science and Technology
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• v.10 no.2
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• pp.83-90
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• 1997

In this paper, optimum extraction condition for berberine which is the indan companent of Coptidis rhizoma was examined at various conditions in the aspect of temperature, solvent and time followed by quantitation with reversed phase HPLC. The efficiency for extraction has been shown the best at $60^{\circ}C$ with 2~3 hours reflux time in methanol or acetic acid. Any significant effect can not be shown from the addition of SLS to extraction solvent.

• Analytical Science and Technology
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• v.22 no.4
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• pp.319-325
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• 2009

An effective and specific procedure for confirmation of neomycin, aminoglycoside antibiotic in honey was developed and validated. Honey was adjusted to pH 2 with 0.1M HCl and applied to weak cation-exchange SPE cartridge. Neomycin was eluted with basified methanol. Following separation by ion-pairing liquid chromatography, neomycin was analysed with positive electrospray ionization and MRM mode. Quantification was linear over the range of $5.0{\sim}250.0{\mu}g/kg$ ($r^2$ >0.9951). The precision (R.S.D.) and accuracy (as a bias) of quality control samples in honey ranged 11.5~18.7% and 10.9~20.9%, respectively. Established method can be applied to analysis of neomycin in honey.

• Journal of the Korean Chemical Society
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• v.33 no.2
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• pp.208-214
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• 1989

A method for the simultaneous determination of copper and cobalt by spectrophotometry has been described. The procedure involves the co-extraction of Cu(Ⅱ) and Co(Ⅱ) from 0.3M HCl into methyl isobutyl ketone as the ion-pairs formed between their thiocyanate complexes and high molecular alkylamines such as Amberlite LA1, Alamine 336, and Aliquat 336. The extract shows the color development to have the maximum absorbances at two different wavelengths i.e., 480 nm for copper and 625 nm for cobalt. Since the spectra of the ion-pairs overlap each other, two simultaneous equations are used to obtain the concentrations from absorbances. Even small amount of Fe(Ⅲ) and Ni(Ⅱ) interferes with the determination of copper. The results of the analysis of samples are in good agreement with the results determined by separate methods within RSD 5.9%.