• Analytical Science and Technology
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• v.8 no.4
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• pp.511-517
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• 1995

A cationic water soluble porphyrin (5,10,15,20-tetrakis (l-methyl-pyridinium-4-yl)porphyrin, $H_2tmpyp^{4+}$) and its metalloporphyrins (MP) were easily extracted into acetonitrile separated by addition of sodium chloride ($4mol\;dm^{-3}$) in the presence of sodium perchlorate, where M denotes $Zn^{2+}$, $Cu^{2+}$, $Co^{3+}$, $Fe^{3+}$, and $Mn^{3+}$ and $P^{2-}$ is porphyrinate ion. The extracted ion-pair complexes were completely dissociated to $[MP(ClO_4)_3]^+$, and $[MP(ClO_4)_2]^{2+}$. The extraction and the dissociation constants were determined by taking into account of the partition constant of sodium perchlorate ($K_D=1.82{\pm}0.01$). The chemical properties of the separated acetonitrile phase as $E_{T(30)}$ and $D_{II,I}$ were determined and compared with other water miscible solvents (acetone, actonitrile, 1,4-dioxane, tetrahydrofuran, 1-propanol and 2-propanol). Furthermore, a sensitive and selective method was proposed for the determination of a subnanogram amount of copper(II) in natural water samples by using the present salting-out method and the porphyrins.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.18 no.4
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• pp.457-464
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• 2020

In this study, extraction of uranium(VI) from an aqueous nitric acid solution was investigated using tri-n-butyl phosphate (TBP) as an extractant in an ionic liquid, 1-alkyl-3-methylimidazolium bis (trifluoromethylsulfonyl)imide ([Cnmim][Tf2N]). The distribution ratio of U(VI) in 1.1 M TBP/[Cnmim][Tf2N] was significantly high when the concentration of nitric acid was low. The value of the distribution ratio decreased as the concentration of the nitric acid increased at lower acidities, and then increased with a nitric acid concentration of up to 8 M. This can be attributed to the different extraction mechanisms of U(VI) based on nitric acid concentrations. Thus, a cation exchange at low acidity levels and an ion-pair extraction at high acidity levels were suggested as the extraction mechanism of U(VI) in the TBP/[Cnmim][Tf2N] system.

• 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.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.

• Journal of Pharmaceutical Investigation
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• v.21 no.3
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• pp.171-177
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• 1991

A reverse-phase, ion-pair high performance liquid chromatographic (HPLC) method for the simultaneous quantative determination of pyridostigmine and its hydrolytic product, 3-hydroxy-N-methylpyridinium (HMP), is descrihed, The assay of pyridostigmine and HMP was linear in the range of amount from 24 to 60 mg/tablet and from 2.4 to 12.0 mg/tablet, respectively, with coefficient of variation (C.V.) of 0.05-0.12% (n=7) and 0.25-0.52% (n=5), respectively, and applicable conveniently even in the case of the mixture of pyridostigmine and HMP. Meanwhile, the conventional UV method gave inaccurate results for the aged pyridostigmine tablets. In the extraction of pyridostigmine from tablets prior to be assayed by HPLC, methanol was found to be more effective than ethanol or distilled water. Multiple extraction (four times) with methanol resulted in the full recovery of pyridostigmine, whereas ethanol gave 95% recovery even after four times extraction. Based on these results. the present method would be very useful for the accurate determination of pyridostigmine in the aged pyridostigmine tablets.

• Journal of Pharmaceutical Investigation
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• v.23 no.3
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• pp.41-50
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• 1993

The iontophoretic delivery across rat skin of quaternary ammonium salts (isopropamide: ISP, pyridostigmine: PS), which are positively charged over a wide pH range, was measured ill vitro. The study showed that: (a) iontophoresis significantly enhanced delivery of ISP and PS compared to respective passive transport; (b) delivery of ISP and PS was directly proportional to the applied continuous direct current density over the range of $0-0.69\;mA/cm^2;$ (c) delivery of ISP and PS was also proportional to the drug concentration in the donor compartment over the range of $0-2{\time}l0^{-2}M:$ (d) sodium ion in the donor compartment inhibited the drug transport possibly due to decreasing the electric transference number of the drug; (e) delivery of ISP and PS increased as the pH of the donor solution increased over the pH range 2-7 suggesting permselective nature of the epidermis, and inhibition of the transference number of the drugs by hydronium ion; (f) some organic anions such as taurodeoxycholate, salicylate and benzoate which form lipophilic ion-pair complexes with ISP inhibited the delivery of ISP. The degree of inhibition by the organic anions was linearly proportional to the extraction coefficient $(K_e)$ of ISP from the partition system with each counteranion between phosphate buffer (pH 7.4) and n-octanol. For PS, however, taurodeoxycholate, but not salicylate and benzoate inhibited the iontophoretic delivery. It suggests that not only sodium ion and hydronium ion but also the counteranions which form lipophilic ion-pairs with quaternary ammonium drugs are not favorable components in formulating the donor solution of the drugs to achieve an effective iontophoretic delivery.

• Journal of the Korean Chemical Society
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• v.55 no.1
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• pp.46-49
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• 2011

A highly sensitive and selective extraction-spectrophotometric method has been developed for determination of trace amounts of cimetidine. This method is based on the extraction of cimetidine as an ion pair with bromothymol blue (BTB) into chloroform and measuring its absorbance at 417 nm. The effect of different variables such as pH, concentration of BTB, volume of chloroform and shaking time was investigated. The effect of interfering ions on the extraction was also studied. The calibration curve was linear in the range of 0.25-8 ${\mu}gmL^{-1}$ with correlation coefficient of 0.9997. The detection limit based on 3Sb was 0.14 ${\mu}gmL^{-1}$ and relative standard deviation for 10 replicated measurements of 1.0 and 4.0 ${\mu}gmL^{-1}$ of cimetidine was 3.2 and 1.49%, respectively. The proposed method was applied to the determination of cimetidine in pharmaceutical samples with good recoveries.

• YAKHAK HOEJI
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• v.31 no.2
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• pp.45-51
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• 1987

Methyl orange(MO) and cetyltrimethylammonium bromide(CTA) were mixed and added to 10ml of the buffer solution and then the solution was shaken for 5 minutes. The maximum absorption wavelength of the reaction product was 419nm. Dichloromethane was the best extracting solvent among the several organic solvents and the most suitable pH range was 2~8. When the CTA-MO calibration curve was made in the best experimental condition, the Lambert-Beer's law was obeyed in the range of CTA concentration of $1.5\times$$10^{-5}$~1.0$\times$$10^{-4}M$ by UV spectrophotometer. This method was possible to determine quaternary ammonium salts in the pharmaceutical preparations.

• Archives of Pharmacal Research
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• v.19 no.5
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• pp.396-399
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• 1996

High-performance liquid chromatographic method with UV detecction was developed for the determination of theophylline and its metabolites in human urine using ${beta}$-hydroxyethyl theophylline$({beta} -HET)$ as an internal standard. For extraction of urine sample, quality control sample and xanthine-free blank urine were mixed with decylamine (ion-paring reagent) and ${beta}$-HET. After saturation with ammonium sulfate, the mixture was then extracted with organic solvent at pH values of 4.0-4.5. All separations were performed with ion-pair chromatography using decylamine as an ion-pairing reagent and 3mM sodium acetate buffered mobile phase (pH 4.0) containing 1% (v/v) acetonitrile and 0.75 mM decylamine. The detection limits of theophylline, 1, 3-DMU, 1-MU, 3-MX and 1-MX in human urine were 0.17, 0.17, 0.39, 0.19 and 0.19 ${\mu}g$/ml, based on a signal-to-noise ratios of 3.0. The mean intraday coefficients of variation (C.V.s) of each compound on nine replicates were lower than 2.0%, while mean interday C.V.s on three days were lower than 1.6%. All separations were finished within 40miutes.

• Journal of the Korean Chemical Society
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• v.27 no.4
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• pp.262-267
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• 1983

A study has been carried out for a scheme of the selective extraction and determination of cesium, sodium and nuclides by the ion association with dicyclohexyl-24-crown-8 and sodium tetraphenylborate from primary coolant of a pressurized water reactor. For that purpose, the effects of hydrogen, cesium and borate ions on the extraction have been investigated. Interferences of iodine and xenon nuclides were found but could be removed by reducing with sodium thiosulfate and back extraction with 1 N hydrochloric acid solution, respectively.