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새로운 HPLC용 형광유도체화제인 1-(N,N-dimethylamino)pyrene-6-sulfonyl chloride를 이용한 아민화합물의 분석
이윤중(Yoon Joong Lee),김용희(Yong Hee Kim),조정길(Jeung Kil Cho) 대한약학회 1991 약학회지 Vol.35 No.4
A new fluorescent derivatizing reagent was developed to be used in HPLC for the trace determination of primary and secondary amines. This new reagent, 1-(N,N-dimethylamino)pyrene-6-sulfonyl chloride, was synthesized by the chlorination of sodium 1-(N,N-dimethylamino)pyrene-6-sulfonate which was obtained from 1-(N,N-dimethylamino)pyrene after sulfonation. Ephedrine and norephedrine were derivatized quantitatively by this reagent. The optimum conditions for the derivatization such as pH, reagent concentration, reaction time and reaction temperature ware examined. The structures of derivatives were identified by IR, 1H-NMR and MS methods. The fluorescence properties and the stability of the derivatives were examined. The derivatives were separated on silica column with an isocratic elution using the mixture of n-hexane and ethylacetate and monitored by fluorescene detector. Linear calibration curves were obtained and detection limits in a 10 mcl injection volume were 5 picomole for ephedrine and norephedrine.
高速液體크로마토그라프法에 의한 錠劑 중 Strychnine Nitrate 및 Yohimbine Hydrochloride 의 同時定量
李允中,曺正吉,李東宣,丁海秀 成均館大學校 科學技術硏究所 1987 論文集 Vol.38 No.1
A simple, rapid extraction and simultaneous determination for yohimbine hydrochloride and strychnine nitrate in tablets, using high performance liquid chromatography with a reverse-phase solvent system, is described. Samples were extracted with 50% methanol by sonication. The extracts were filtrated and applied to HPLC. HPLCs of yohimbine hydrochloride and strychnine nitrate were carried out on μ-Bondapak C_18 Radial-pak cartridge(8mm i.d. x 10 cm) and CH_3CN/H_2O/CH_3COOH=20/78/2 for the solvent system. Recoveries from model preparations were more than 98%. This method was considered to be useful for the determination of yohimbine hydrochloride and strychnine nitrate in tablets at the same time.
李允中,曺正吉,丁海秀,嚴東玉 成均館大學校 科學技術硏究所 1988 論文集 Vol.39 No.2
A highly sensitive and selective fluoresence high-performance liquid chromatography using 1-bromoace-tylpyrene as a pre-labelling reagent was applied to the determination of cinnamic acid and glycyrrhetic acid at p mol level. The optimum conditions for the derivatization such as concentrations of KOH, 18-crown-6, and 1-bromoacetylpyrene, reaction temperature and reaction time were investigated. The derivatives were separated on a reversed phase column using the mixture of acetonitrile, methanol and water as the mobile phase. The effluent was menitored by fluorometer. Linearities of calibration curve were obtained between 0.5 p mol and 2.0 p mol. The detection limit of cinnamic acid and glycyrrhetic acid was 0.05 p mol in a 20 ㎕ of injection volume.
高速液體 Chromatography에 의한 製劑中 Crotamiton의 分離定量에 관한 硏究
李允中,曺正吉,李東宣,尹汝生,金在鉉 成均館大學校 科學技術硏究所 1983 論文集 Vol.34 No.1
The method for rapid determination of crotamiton in ointment and action was established by using reverse phase high performance liquid chromatography. First, crotamiton in ointment (or lotion) was extracted with methanol and 20㎕ portion of the extracted solution was injected into the column. The effluent was monitored by an ultraviolet detector at 254 um. On a μ-Bondapak C_18 column(3.9 mm i. d x 30cm) with an eluent of MeOH/H_2O=55/45, a sufficient separation of crotamiton, preservatives, and minor components was obtained. The proposed procedure provided an accurate, sensitive, and rapid estimation, and a good , ability suggesting a suitable assay method for crotamiton in pharmaceuticals.
李允中,曺正吉,朴元敎,李康春 成均館大學校 科學技術硏究所 1988 論文集 Vol.39 No.1
A simple and highly sensitive method for the determination of unsaturated fatty acids (C_16:1, C_20:4, C_20:5) is described. I-Bromoacetylpyrene was used as the pre-column fluorescent labelling reagent for HPLC. Fatty acids were derivatized quantitatively into fluorescent compounds by treating with 1-bromoacetylpyrene in the presence of 18-crown- 6 in acetonitrile. The optimum conditions for the derivatization such as, concentrations of KOH, 18-crown-6, and 1-bromoacetylpyrene, reaction temperature and reaction time, were investigated. The derivatives were separated on a reversed phase column (LiChrosorb RP-8, 5 ㎛) using the tertiary mixture of acetonitrile, methanol, and water as the mobile phase. The effluent was monitored by fluorometer (excitation wavelength; 366 nm, emission wavelength; 454 nm). Linearities of calibration curve were obtained between 5.0 p mol and 40.0 p mol. The detection limit of fatty acids was 1 p mol in a 20μl of injection volume.
2-Bromoacetylnaphthalene을 螢光誘導體化劑로 利用한 Alclofenac의 HPLC 分析에 관한 硏究
李允中,曺正吉,河仁植,金容熙 成均館大學校 科學技術硏究所 1990 論文集 Vol.41 No.1
A simple, rapid and high sensitive method for determination of alclofenac is described. 2-Bromoacetylnaphthalene was used as the pre-column fluorescent derivatizing reagent for high performance liquid chromatography. Alclofenac was derivatized quantitatively into fluorescent compound by reacting with 2-bromoacetylnaphthalene in the presence of 18-crown-6 ether in acetonitrile. The optimum conditions for the derivatization such as concentration of KOH, 18-crown-6 and 2-bromoacetylnaphthalene, reaction temperature and reaction time were investigated. The structure of alcolofenac derivative was confirmed from IR, NMR and mass spectra. The fluorescence properties of alclofenac derivative were examined. The derivative was separated on a reverse phase column (Lichrosorb RP-8) in isocratid elution mode using the secondary mixture of acetonitrile and water as the mobile phase. The effluent was monitored by fluorometer.(Ex. 303, Em. 418 nm). The calibration plots for the peak area versus concentration of alclofenac observed to be linear(r =0.999).
2-Bromoacetylnaphthalene을 螢光誘導體化劑로 利用한 Ibuprofen의 HPLC 分析에 관한 硏究
李允中,金容熙,曺正吉,禹炳虎 성균관대학교 약학연구소 1990 成均藥硏論文集 Vol.2 No.1
Abstract-A simple, rapid and high sensitive HPLC method for determination of ibuprofen is investigated. 2-Bromoacetylnaphthalene was used as the pre-column fluoresent derivatizing reagent for high performance liquied chromatography. Ibuprofen was derivatized quantitatively into fluorescent compound by reacting with 2-bromoacetylnaphthalene in the presence of 18-crown-6 ether in acetonitrile. The optimum conditions for the derivatization such as concentration of KOH, 18-crown-6 and 2-bromoacetylnaphthalene, reaction temperature and reaction time were investigated. The structure of ibuprofen derivative was confirmed from IR, mass spectra. The fluorescence properties of ibuprofen derivative were examined. The derivative was separated on a reverse phase column in isocratic elution mode using the secondary mixture of acetonitrile and water as the mobile phase. The effluent was monitored by fluorometer. The calibration plots for the peak area versus concentration of ibuprofen observed to be linear.(r=0.999)
李允中,申秉澈,曺正吉,李東宣 成均館大學校 科學技術硏究所 1989 論文集 Vol.40 No.1
A simple, rapid and high sensitive method for the determination of prostaglandin F_2α (C_20H_34O_5) is described. 1-bromoacetylpyrene was used as the pre-column fluorescent derivatizing reagent for high performance liquid chromatography. PG F_2α was derivatized quantiatively into fluorescent compound by reacting with 1-bromoacetylpyrene in the presence of 18-crown-6 in acetonitrile. The derivative was separated on a normal phase column in isocratic elution mode using the secondary mixture of chloroform and tetrahydrofuran as the mobile phase. The effluent was monitored by fluorometer. The calibration plots for the peak heights versus concentrations of PG F_2α were observed to he linear.