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이온쌍-고성능 액체크로마토그래피에 의한 감기약 시럽에서 타르색소 첨가물의 동시분석
김경옥(Jing Yu Jin),황호(Hu Huang),이범규(Beom-Gyu Lee),이원재(Wonjae Lee) 한국생물공학회 2010 KSBB Journal Vol.25 No.5
A simple and efficient analytical method for the simultaneous determination of seven tar color additives was developed using ion pair high performance liquid chromatography. The conditions for HPLC analysis were as follows: column, μ-Bondapak C18 (10 μm, 300 × 3.9 mm i.d.); gradient mobile phase, 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrile-methanol (65:25:10) as a mobile for fraction A and 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrilemethanol (40:50:10) as a mobile for fraction B; flow rate, 1.0 mL/ min; detection wavelength, 254/520/620 nm. We could attain to the detection limits as 0.01~0.05 μg/mL (254 nm) and 0.005~0.01 μg/mL (520 nm) for six red tar color additives, and 0.05 μg/mL (254 nm) and 0.002 μg/mL (620 nm) for Fast green FCF. This analytical method was applicable to determine the tar color additives contained in several commercial cold syrups.
UV-VIS 분광기기의 성능검증을 위한 밸리데이션 가이드라인의 제정 및 응용
김경옥(Jing Yu Jin),강영구(Young Koo Kang),이원재(Wonjae Lee) 대한약학회 2006 약학회지 Vol.50 No.3
For the increasing demand for the validation of analytical results, one of the important concerns of the analyst is to be assured that the instrumentation is working to qualified conditions. In this study, we have investigated and compared several validation guidelines of the performance verification of UV-VIS spectrophotometer used in pharmacopoeias of major countries and UV-VIS instrument analytical companies, and we proposed the practically useful validation guidelines of UV-VIS spectrophotometer. Based on our proposed validation guidelines of UV-VIS spectrophotometer, several UV-vis spectrophotometers used in drug manufacturing laboratories were validated for their performances.
다당 유도체를 기초로 한 키랄 컬럼에서 아미노산 에스테르의 안트르알디민 유도체의 광학분리 및 광학순도 측정
황호(Hu Huang),김경옥(Jing Yu Jin),이원재(Wonjae Lee) 한국생물공학회 2011 KSBB Journal Vol.26 No.2
The chromatographic enantiomer separation of 9-anthraldimine derivatives of α-amino acid methyl and ethyl esters on four polysaccharide based chiral columns was performed. The 9-anthraldehyde Schiff base derivatives of α- amino acid esters were readily synthesized by stirring the α-amino acid ester hydrochloride salts with 9-anthraldehyde in the presence of 1,8-diazabicyclo [5.4.0]undec-7-ene as a base and anhydrous MgSO₄. Chiralcel OD or Chiralcel OD-H showed the greatest enantiomer resolution of 9-anthraldimine derivatives of α-amino acid methyl and ethyl esters. The L-enantiomers of all the analytes were preferentially retained on Chiralcel OD or Chiralcel OD-H. This analytical method was applied in the determination of optical purities of several commercially available D- or L-α-amino acid methyl esters.
고성능 액체 크로마토그래피에 의한 다당 유도체를 기초로 한 흡착되거나 공유결합된 키랄 고정상에서 키랄 아미노 알코올의 안트르알디민 유도체의 광학분리
서문준(Wen Jun Xu),김경옥(Jing Yu Jin),이원재(Wonjae Lee) 한국생물공학회 2011 KSBB Journal Vol.26 No.4
The convenient derivatization method of chiral amino alcohols as 9-anthraldimine Schiff base derivatives for chiral resolution was developed and the liquid chromatographic enantiomer separation of chiral amino alcohols as 9-anthraldimine derivatives was investigated on several coated and covalently bonded polysaccharide-derived chiral stationary phases (CSPs). In general, the performance of Chiralcel OD-H (or Chiralcel OD) (α = 1.24-2.89), the coated CSP derived from cellulose derivative was superior to the other CSPs for resolution of 9-anthraldimine derivatives of several amino alcohols. The results of enantioseparation depending on the structure of 9-anthraldimine analytes like the steric bulky group and the polar moiety etc were discussed. The analytical method was applied to measure the enantiomeric purity of commercially available chiral amino alcohols. It is expected that the convenient analytical method will be very efficient for determination of enantiomeric purity of amino alcohols as 9-anthraldimine Schiff base derivatives with strong UV absorption.