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Picric acid를 전자수용체로 한 Phenothiazine계 화합물의 정량법
옥치완,신태용 대한약학회 1987 약학회지 Vol.31 No.5
A rapid and sensitive spectrophotometric method has been developed for quantitation of some phenothiazine derivatives (PTZDS). The method depends on the formation of insoluble yellow complexes between PTZDS and picric acid (PCA) in aqueous layer. These complexes are quantitatively extracted from aqueous phase into chloroform. The binding ratio of PTZDS-PCA complexes were presumed as PTZDS-1 to PCA-1 by means of mole ratio and continuous variation methods. The complexes are stable for more than 24hours in chloroform layer at room temperature. Most of compounds associated with pharmaceutical preparation of PTZDS do not interfere with this method. However, chlorpheniramine and diphenhydramine interfere with the riaethod. The binding state of PTZDS-PCA complexes were presumed by IR and $^1$H-NMR spectra as intermolecular hydrogen bonding.
전하이동 착물형성에 의한 Ephedrine Alkaloids의 분석화학적 연구
옥치완,백채선 대한약학회 1987 약학회지 Vol.31 No.5
The weak UV absorbing ephedrine alkaloids such as ephedrine, pseudoephedrine, methylephedrine and norephedrine could be analyzed by charge-transfer spectrophotometric method. The results obtained are summarized as follows: (1) It was possible to determine a weak UV absorbing ephedrine alkaloids using the intense charge-transfer UV bands in chloroform. (2) This method was suitable for the spectrophotometric determination of ephedrine alkaloids in mixed pharmaceutical preparation. (3) Linear relationship was found between absorbance and concentration in the range of 1.0$\times$$10^{-5}M$~5$\times$$10^{-5}M$ of ephedrine ($\varepsilon$= 2.72$\times$$10^{4}LM^{-1}cm^{-1}$ and pseudoephedrine ($\varepsilon$=2.84$\times$$10^{4]LM^{-1}cm^{-1}$), 1.0$\times$$10^{-5}M$~5$\times$$10^{-5}$M of methylephdrine ($\varepsilon$=1.68$\times$$10^{4}LM^{-1}cm^{-1}$) and 1/3$\times$$10^{-4}M$~4/3$\times$$10^{-4}M$ of norephedrine ($\varepsilon$=0.74$\times$$10^{4}LM^{-1}cm^{-1}$. (4) CT- complex of ephedrine, pseudoephedrine and methylephedrine has absorption maxima at 293nm and norephedrine have absorption maximum at 253nm. (5) CT-complexes were formed in a 1:1 ratio between ephedrine alkaloids and iodine in chloroform. (6) By UV, IR, and $^1H$-NMR spectra, it could be inferred that CT-complexes were formed by interaction between the basic nitrogen of ephedrine alkaloids as electron (n) donor and iodine as electron ($\sigma$) acceptor.
HPLC법에 의한 1,2-디아미노-4,5-메틸렌디옥시벤젠을 형광유도체화제로 한 혈청 및 뇨 중의 alpha-케토산의 분석
옥치완(Chi Wan Ok),김대기(Dae Ki Kim),박송자(Song Ja Park),박종세(Jong Sei Park) 대한약학회 1992 약학회지 Vol.36 No.4
A simple and sensitive high performance liquid chromatographic method to quantitate alpha-keto acids in serum and urine was investigated. alpha-Keto acids react with 1,2-diamino-4,5-methylenedioxybenzene (DMB) in the presence of 2-mercapto-ethanol and sodium hydrogen sulfite to form highly fluorescent derivatives, substituted 6,7-methylenedioxyquinoxalinol. The derivatization procedure was performed in water bath at 100oC , and completed within 50 min. By the use of a reversed-phase column and multi-step gradient with two solvents, a mixture containing twelve of these derivatives were efficiently resolved within 35 minutes. The optimal wavelength of the fluorescence detector are lambdaex = 364nm and lambdaem = 445nm. The quantitation of the individual alpha-Keto acids was reproducible with relative standard deviation of 3.0~7.9% and had a detection limits of 10~60 fmol, except for p-hydroxyphenylpyruvic acid (960 fmol).
Charge Transfer Complex 形成에 의한 鹽酸테트라하이드로졸린의 吸光度 定量法
玉致完,宋在益 圓光大學校 1990 論文集 Vol.24 No.2
The intense absorption band in UN region of charge transfer complex of tetrahydrozoline with iodine in chloroform medium were utilized in a sensitive spectrophotometric determination of tetrahydrozoline hydrochloride. Alkaline aquous solution of tetrahydrozoline hydrochloride were extracted throughly to chloroform ?? tetrahydrozoline base, the layer is mixed with iodine in chloroform, and formed charge transfer complex of faint yellow solution showed absorption maxima at 293nm. Quantification range of tetrahydrozoline hydrochloride is 7.5×??mole∼1.35×10??mole at the absorption maxima. The binding ratio of this charge transfer complex were determined as tetrahydrozoline base-1 by means of mole ratio and continuous variation methods. The methods can be applied to quantitative analysis of tetrahydrozoline hydrochloride containing chloroform extracts obtained in pharmacopoeial assays.