• 분석과학
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• 제8권4호
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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.

• 방사성폐기물학회지
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• 제18권4호
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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.

• 분석과학
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• 제6권3호
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• pp.289-296
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• 1993

자연수 중 극미량 몰리브덴[Mo(VI)]을 분리 정량하기 위하여 Mo(VI)의 킬레이트이온을 이온쌍으로 만들어 유기용매로 상승 용매추출시키는 방법에 대해 검토하였다. 자연수 시료 100mL를 분별 깔때기에 취하였다. pH 4.0인 시료에 0.01M alizarin red S 용액 0.5mL를 가하여 Mo(VI)-ARS의 킬레이트이온을 형성시킨 다음, aliquat-336을 0.2% 되게 녹인 chloroform 10mL를 가해 30초 정도 격렬하게 흔들어 모든 킬레이트이온이 이온쌍을 형성하여 용매층으로 분배되도록 하였다. 90분간 방치하여 두 쌍이 완전히 분리되면 chloroform층을 받아서 520nm에서 흡광도를 측정하여 검정곡선법으로 Mo(VI)을 정량하였다. 이상의 과정에서 용액의 pH, alizarin red S와 aliquat-336의 가해 주는 양, 흔들어 주고 방치하는 시간 등과 같은 추출조건에 대해서 검토하였다. 실제 시료인 강물과 수돗물의 분석에 응용하였다. 이들 시료에 Mo(VI)을 일정량 가하여 분석한 회수율은 모두 99% 이상으로 본 방법이 정량적임을 확인하였다.

• 분석과학
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• 제6권3호
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• pp.329-334
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• 1993

형성시킨 Mo(VI)의 킬레이드이온과 이온쌍을 만들어 유기용매에로 상승추출시켜 자연수 중 극미량의 몰리브덴[Mo(VI)]을 분리 정량하는 방법을 해수에 응용하였다. pH 2.0과 4.0에서 anthranilic acid를 가해 Cu(II)와 Fe(III), Zn(II)을 침전시켜 그들의 방해를 제거한 해수시료 100mL를 분액 깔때기에 취하였다. pH를 4.6으로 조절한 시료에 0.01M alizarin red S 1.0mL를 가하여 Mo(VI)-ARS의 킬레이트이온을 형성시킨 다음 aliquat-336을 0.6% 되게 녹인 chloroform 10mL를 가해 30초 정도 격렬하게 흔들어 모든 킬레이트이온이 이온쌍을 형성하도록 하였다. 30분간 방치하여 두 상이 완전히 분리되면 chloroform층을 받아서 520nm에서 흡광도를 측정하여 검정곡선법으로 Mo(VI)을 정량하였다. 이상의 과정에서 추출조건인 용액의 pH, alizarin red S와 aliquat-336의 가해 주는 양, 흔들어 주고 방치하는 시간 등과 공존 이온들의 방해와 제거방안에 대해서 검토하였다. 실제 시료인 동해와 황해 해수의 분석에 응용하였으며, 이들 시료에 Mo(VI)을 일정량 가하여 분석한 회수율은 모두 85% 이상으로 본 방법을 해수 중 Mo(VI)의 분석에서도 정량적임을 확인하였다.

• Journal of Pharmaceutical Investigation
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• 제21권3호
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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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• 제23권3호spc1호
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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.

• 대한화학회지
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• 제55권1호
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• pp.46-49
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• 2011

감도가 높고 선택적인 추출-분광광도법은 미량의 시메티딘의 측정을 위해 개발되어 왔다. 이 방법은 클로로포름안에 브로모티몰 블루(BTB)와 함께 이온 쌍으로 시메티딘의 추출에 기초했다. 그리고 417 nm에서 흡광도를 측정하고 있다. pH, BTB의 농도, 클로로포름의 부피, 섞는 시간과 같은 다른 변수들의 효과를 연구하였다. 또한, 추출에서 간섭이온의 효과도 연구하였다. 보정곡선은 0.9997의 상관계수와 함께 0.25~8 ug/mL의 범위에서 선형이다. 3Sb에 기초한 검출한계는 0.14 ug/mL이고 시메티딘의 0.1과 4.0 ug/mL의 10번 측정에 대한 상대표준편차는 3.2와 1.49%이었다. 제안된 방법은 좋은 회수와 함께 약제 샘플에서 시메티딘의 측정에 적용되었다.

• 약학회지
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• 제31권2호
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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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• 제19권5호
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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.

• 대한화학회지
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• 제27권4호
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• pp.262-267
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• 1983

가압형 경수로의 일차 냉각수로부터 세슘 핵종을 선택적으로 분리하여 그 방사능을 결정하기 위한 Scheme이 연구되었다. 세슘의 분리는 dicyclohexyl-24-crown-8과 sodium tetraphenylborate에 의한 이온쌍 용매추출에 의해서 이루어졌으며 추출에 미치는 수소, 세슘, 나트륨 및 borate 이온의 영향이 연구되었다. 요오드와 크세논 핵종의 방해 현상은 각각 티오황산나트륨에 의한 요오드의 환원과 1N 염산수용액에 의한 역추출에 의해서 제거될 수 있었다