• Bulletin of the Korean Chemical Society
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• 제31권10호
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• pp.2813-2818
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• 2010

A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion ($TBA^+$)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a $100\;{\mu}L$ micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = $1.0{\times}10^{-4}\;M$, [$TBA^+$] = $2.0{\times}10^{-2}\;M$, [$CHCl_3$] = $100.0\;{\mu}L$ and [$ClO_4$] = $2.0{\times}10{-2}\;M$, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results.

• Bulletin of the Korean Chemical Society
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• 제32권3호
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• pp.768-778
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• 2011

Calixpyrroles and related macrocycles are non-planer synthetic anion receptors that have attracted considerable attentions in recent years. Although the synthesis of calix[4]pyrrole (known as meso-octamethylporphyrinogen) was reported more than 100 years ago, the anion binding properties were first discovered in 1996. The simple calix[4]pyrroles can be synthesized in single step in high yield by condensation of pyrrole with acetone. The compounds showed preferential binding for halide anions including fluoride, phosphate, carboxylate, and chloride in organic media. Efforts to improve the anion affinity of calix[4]pyrrole and to enhance its selectivity have led to the synthesis of a variety of new calixpyrrole derivatives. Among the various modifications, introduction of straps on one side of the calix[4]pyrroles are the most effective. Incorporation of aromatic rings other than pyrroles also exhibited interesting binding behaviour. Introduction of signalling units as part of the strapping element enable to detect the anions on chromogenic or fluorogenic fashion. Finding of the anion transport properties across the membrane and cytotoxic effects of the calix[4]pyrroles open new window for calixpyrrole-related research. The polymer-incorporated systems have also been employed as anion complexants in solvent-solvent extraction. These old, yet easy-to-make macrocycles have well advanced more recently with the discovery of the ion-pair complexation properties. In this review, the synthetic developments and anion binding properties of calixpyrroles for the last decades will be discussed and will cover the advances in calixpyrrole chemistry.

• 약학회지
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• 제37권1호
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• pp.30-35
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• 1993

HPLC/fluorescence detection method for the analysis of pancuronium bromide in biological fluids was developed. The method depends on the formation of insoluble red complex between pancuronium bromide and rose bengal in aqueous layer. This complex is quantitatively extracted from aqueous layer into chloroform layer. The complex is stable for 1 day in chloroform layer at room temperature. It was possible to analyze pancuronium bromide in the range of 0.05~0.5 $\mu\textrm{g}$/ml without the effect of co-prescribed drugs.

• 공업화학
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• 제30권1호
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• pp.34-38
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• 2019

탄산화 공정을 위한 Ca 추출원으로 시멘트 산업부산물을 사용하였다. ICP와 XRD 분석을 통하여 시멘트 산업부산물은 대부분 CaO와 KCl로 구성되어 있음을 확인하였다. 최적화된 추출용제의 종류 및 농도는 1.5 M of hydrochloric acid이며 최적의 고액비는 0.1 g/mL이었다. 추출 성능 실험 결과를 통해 양이온의 추출효율은 이온 결합 형태 및 용해도에 의존함으로 판단되었다. 또한 추출 공정 후, 첨가물의 종류 및 주입 순서에 따라 선택적으로 양이온이 분리될 수 있음을 확인하였다. pH를 9.5, 13으로 조절하기 위하여 NaOH를 주입하였을 때 불순물과 $Ca(OH)_2$가 침전되었으며, $C_2H_5OH$를 주입한 경우 KCl 형태로 분리된 K가 침전되었다.

• 약학회지
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• 제16권4호
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• pp.180-185
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• 1972

A new spectrophotometric method was established for the determination of undecylenic acid. The method is based on the solvent extraction into nitrobenzene of the ion pair formed between tris(1,10-phenanthroline)Fe(II) chelate and the anion of undecylenic acid. The maximum absorbance of the extract in the organic phase was at 518nm. A maximum extraction was obtained at pH 9-11, when excess of at least 50-fold(molar) of the phenanthroline-Fe(II) chelate to undecylenic acid was present. The color intensity of the extracted species remained constant at room temperature for the several hours after separation of the organic layer. A linear relationship was obtained over the tested range of 5-20${\gamma}$/ml of undecylenic acid. The effect of several other fungicids on this method was investigated. The method was applied to the determination of undecylenic acid in preparations and the results were in good agreement with those added amounts.

• 분석과학
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• 제26권3호
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• pp.182-189
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• 2013

본 연구에서는 HPLC-ICP-MS를 이용하여 여러 식품에 포함된 셀레늄의 화학종을 분리하고 정량 하였다. 양이온 교환 크로마토그래피를 사용할 때에 무기셀레늄 화학종의 분리는 효율적이나 유기셀레늄 화학종은 분리가 완전하지 못한 반면, 역상 이온쌍 크로마토그래피에서는 유기와 무기 셀레늄 화학종들을 모두 잘 분리 할 수 있었다. $C_8$ 컬럼($Symmetryshield^{TM}\;RP_8$, 3.5 ${\mu}m$, $4.6{\times}150$ mm)을 이용하여 최적조건(이동상; 5% 메탄올, ion-pairing reagent; 0.05% nonafluorovaleric acid, 흐름속도; 0.9 mL $min^{-1}$)하에서 표준물 Se(IV), Se(VI), SeCys (selenocystein), SeMet (selenomethionine), Se-M-C (seleno methyl cystein)를 성공적으로 분리하였다. 시료에서의 셀레늄화학종의 추출은 마이크로파를 이용한 추출과 효소(protease I, trypsin, protease XIV)를 이용한 추출을 사용하였는데 시료에 따라 서로 다른 효율과 결과를 보여주었다. 식물성 시료인 마늘 시료는 protease I, 동물성 시료인 돼지고기와 고등어 시료는 protease I + trypsin이 가장 효율적인 추출을 보여주었다. 각 시료의 최적 조건을 선택하여 셀레늄 화학종을 추출하고 분리 정량한 결과 이들에는 주로 무기 Se, SeCys, SeMet이 수 ${\mu}g$ $g^{-1}$ 내지 수 십 ${\mu}g$ $g^{-1}$ 수준으로 포함되어 있음을 알 수 있었다.

• 대한방사성의약품학회지
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• 제2권2호
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• pp.84-95
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• 2016

Considerably increasing interest in using the theranostic isotopes/ isotope pairs of radiometals like $^{44/47}Sc$ and $^{64/67}Cu$ for diagnosis and/or therapeutic applications in the nuclear medicine procedures necessitates its reliable production and supply. Separation and purification of no-carrier-added (NCA) isotopes from macro quantitates of the irradiated target matrix along with other impurities is a cardinal procedure amongst several other steps involved in its production. Multitudinous methods including but not limited to liquid-liquid (solvent) extraction, extraction chromatography (EXC), ion exchange, electrodeposition and sublimation are routinely applied either solitarily or in combination for the separation and purification of radioisotopes depending on their production routes, radioisotope of interest and impurities involved. However, application of EXC though has shown promises towards the numerous separation techniques have not received much attention as far as its application prospects in the field of nuclear medicine are concerned. Advances in the recent past for application of the EXC resins in separation and purification of the several medically important radioisotopes at ultra-high purity have shown promising behavior with respect to their operation simplicity, acidic and radiolytic stability, separation efficiencies and speedy procedures with the enhanced and excellent extraction abilities. In this mini review we will be talking about the recent developments in the application and the use of EXC techniques for the separation and purification of $^{44/47}Sc$ and $^{64/67}Cu$ for medical applications. Furthermore, we will also discuss the scientific and practical aspects of EXC in the view of separation of the NCA trace amount of radionuclides.

• 한국의류학회지
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• 제24권3호
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• pp.422-428
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• 2000

At present, analytical methods available for determining the amount of cationic surfactants(DSDMAC) on the fabrics are spectrophotometric method based on formation and extraction of the colored ion pair with anionic dye, radiochemical analysis and HPLC analysis. This study presents new analytical methods based on the formation of cationic surfactant(DSDMAC)-disulfine blue complex on the cotton fabric. Test methods for determining the amount of DSDMAC-disulfine blue complex on the cotton fabrics are measuring the reflectance of the colored fabric and the absorbance of the methanol solution of DSDMAC-disulfine blue complex extracted from dyed cotton fabric. Linear relationships between the K/S value of the fabric treated with DSDMAC followed by disulfine blue and the amount of DSDMAC sorbed by cotton fabric were obtained. Thus, the amount of DSDMAC sorbed by cotton fabric can be determined by K/S value of the fabric. DSDMAC-disulfine blue complex on the cotton fabric was extracted with methanol. The amount of DSDMAC sorbed by cotton fabric was estimated by measuring the absorbance of the methanol solution extracted from dyed cotton fabric.

• Journal of Pharmaceutical Investigation
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• 제11권3호
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• pp.1-13
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• 1981

A new application of monoacidic dye is reported for the determination of pipethanate hydrochloride(PTH). The method is based on solvent extraction into chloroform of an ion-pair compound formed between methyl orange(MO) and PTH. PTH is determined by measuring absorbance of the extracts over the range of $2.0{\sim}12.0{\mu}g/ml$ at 420nm. Best accuracy can be obtained for solutions containing $3.0{\sim}8.0{\mu}g/ml$. The color was stable for at least 5 days. The molar absorptivity was $2.88\;{\times}\;10^4\;l,\;mol^{-1},\;cm^{-1}$. Molar ratio and continuous variation plots have a maximum at 0.5 mol fraction of MO, indicating a 1 : 1 MO-PTH ratio.

• 약학회지
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• 제38권4호
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• pp.379-388
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• 1994

A new method for the analysis of metocurine iodide in biological fluids was developed. Metocurine iodide was quantitatively extracted with rose bengal from aqueous layer into dichloromethane layer and the amount of metocurine iodide was calculated from the amount of rose bengal which was determined by HPLC with fluorescence detector. It was possible to analyze metocurine iodide without the effect of co-prescribed drugs in the concentration range of $0.09{\sim}9.10\;{\mu}g/ml$. The detection limits of metocurine iodide in urine and blood were 0.8 and 1.2 ng at S/N=3, each respectively.