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백만정,김경례 대한약학회 2004 Archives of Pharmacal Research Vol.27 No.5
An efficient analytical method was devised for the accurate L-muscone assay in aqueous samples. It involves solid-phase extraction of L-muscone in adsorption mode using XAD-4 as the sorbent and dichloromethane modified with 10% (v/v) methanol as the eluting solvent. The gas chromatographic analysis of the eluate residue dissolved in toluene on a DB-5MS capillary column provided complete resolution of L-muscone from the co-extracted interferences. The overall method showed excellent linearity (r2 ³ 0.9994) in the range of 0.1 to 2.0 mg/mL with good intra- and inter-day precisions (% RSD = 2.5~7.3) and with high extraction recovery rates (³ 98.1%). When the present method was applied to a L-muscone herbal drink product, the within-batch RE (%) in the labeled concentration (1.5 mg/mL) for the three randomly chosen bottles were -2.4, -1.3 and -3.3 with high precision (% RSD £ 3.1). The present method is considered to be suitable for quality control evaluation on liquid drinks and other complex formulations fortified with L-muscone.
백만정,Duc-Toan Nguyen,김경례 대한약학회 2004 Archives of Pharmacal Research Vol.27 No.12
The enantiomeric composition tests on flurbiprofen and ketoprofen present in patch products and in urine excretions following patch applications were performed as diastereomeric (R)-(+)- 1-phenylethylamides by achiral gas chromatography and by gas chromatography-mass spectrometry in selected ion monitoring mode. The method for determination of (R)- and (S)-enantiomers in the range from 0.1 to 5.0 μg was linear (r ≥ 0.9996) with acceptable precision (% RSD ≤ 5.2) and accuracy (% RE = 0.6 ~ -2.4). The enantiomeric compositions of flurbiprofen in one patch product and of ketoprofen in five different products were identified to be racemic with relatively good precision (≤ 6.4%). The urinary excretion level of (R)-flurbiprofen was two times higher than its antipode, while the comparable excretion levels of (R)- and (S)-enantiomers for ketoprofen were observed.
Chiral Profiling Analysis of β-Blockers by Capillary Electrophoresis Using Dual Chiral Selectors
백만정,김경래,이원재 대한화학회 2015 Bulletin of the Korean Chemical Society Vol.36 No.5
Simultaneous analysis of several β-blockers using a novel dual chiral selector system was achieved for their accurate chiral discrimination by chiral capillary electrophoresis (CE) in normal polarity mode. The CE system was operated using heptakis(2,6-di-O-methyl)-β-cyclodextrin (DM-β-CD) dissolved in 100 mM phosphoric acid–triethanolamine buffer (pH 3) and (+)- or (−)-18-crown-6-tetracarboxylic acid (18-C-6-TA) as a co-chiral selector in DM-β-CD solution. All eight investigated analytes were resolved using (+)-18-C-6-TA as a co-chiral selector in the presence of DM-β-CD solution, whereas the other β-blockers, except propranolol, were resolved using (−)-18-C-6-TA as the second chiral selector in DM-β-CD solution. Also, DM-β-CD had a major effect on chiral discrimination compared with 18-C-6-TA as a co-chiral selector. Relative migration times to that of (S)-pindolol as an internal standard were characteristic of each enantiomer with good precision. The method showed good linearity with a correlation coefficient (r ≥ 0.993). The precision as a percentage of relative standard deviation (% RSD) and accuracy as a percentage of relative error (% RE) ranged from 0.5 to 9.6 and from −5.7 to 9.1, respectively. These were adequate for the chiral assay of the β-blockers investigated. Thus, the present chiral profiling method is expected to be useful for accurate chiral discrimination and optical purity tests of chiral β-blockers and their related drugs.
고성능 액체크로마토그래피의 다당유도체를 기초로 한 키랄 고정상에서 이동상 첨가제가 키랄 아민의 광학분리에 미치는 영향
백만정(Man-Jeong Paik),윤혜란(Hye-Ran Yoon),이원재(Wonjae Lee) 한국생물공학회 2014 KSBB Journal Vol.29 No.3
Chromatographic enantiomer resolution of chiral amines was performed on several covalently immobilized and coated chiral stationary phases (CSPs) based on polysaccharide derivatives under the mobile phase conditions containing base or acid or acid/base additive. The chromatographic parameters including separation factors and capacity factors were greatly influenced by the nature of the mobile phase containing base or acid or salt additive as well as the used CSPs. When 0.05% triethylamine/0.05% trifluoroacetic acid as an additive in the mobile phase was used on all CSPs in this study, the greatest enantiomer resolution was observed except for Chiralpak AD. Also, it was shown that the change of base additive into acid or salt in the mobile phase may directly affect chiral recognition mechanisms between the chiral selectors and analytes occurring during enantiomer separation, resulting in the change of elution orders.