• 분석과학
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• 제11권6호
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• pp.429-435
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• 1998

유리 담즙산 및 담즙산의 글리신복합체를 dansyl cadaverine을 형광유도체화제로 사용하여 역상HPLC에서 분리하고 형광으로 검출할 수 있는 방법을 개발하였다. 8종류의 유리 및 복합체 담즙산을 dimethylformamide를 반응용매로 하여, amide결합 형성반응용 축합제로서 diethyl phosphorocyanidate를 사용하여 형광유도체화제인 dansyl cadaverine과 반응시켰다. 반응액중 일부를 20% methanol-water/acetonitrile을 기본 용리액으로한 직선 농도구배 조건의 HPLC에 의하여, 8가지 담즙산류를 완전히 분리할 수 있었다. 역상컬럼으로부터 용출된 담즙산의 형광유도체는 여기파장(${\lambda}ex.$) 340 nm, 형광파장 (${\lambda}em.$) 520 nm에서 측정하여 콜린산의 경우 약 10 pg(S/N 비=5)까지 측정할 수 있었다.

• Archives of Pharmacal Research
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• 제22권3호
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• pp.294-299
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• 1999

Precolumn orthophthaldehyde (OPA) labeling method of sphingoid bases, sphingosine and sphinganine, was investigated to obtain high fluorescent detectability. In order to improve the fluorescent yield, we investigated the optimal solubility of sphingoid bases for five pre-incubation solvents by incorporating the heating procedure before OPA derivatization. The pre-incubation in ethanol prominently increased the fluorescent peak height of OPA derivative for each sphingoid bases in high performance liquid chromatography. About tenfold increase of detectability was archived by pre-incubating lipid extracts pellets in ethanol at $60^{\circ}C$ for 30 min. Optimal derivatization was performed in 30 min at ambient temperature and the fluorescent intensity of OPA derivative was stable for two weeks at $4^{\circ}C$. The detection limit of sphingosine was 0.1 pmol as injected amount. This method was applied to the determination of cellular sphingosine and sphinganine in various human lung cancer cells. This OPA procedure was prospective to be useful for quantitating the amount of sphingoid bases in other cancer cells.

• 한국해양바이오학회지
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• 제15권2호
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• pp.96-102
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• 2023

Salicornia herbacea, a noted halophyte, has been widely researched for its diverse physiological activities. The continuous exploration of its compounds is essential. This study employed gas chromatography (GC) coupled with mass spectrometry (MS) for qualitative analysis. This involved pretreatment including trimethylsilyl (TMS) derivatization of the S. herbacea extract, facilitating its GC analysis. Five compounds, including various fatty acids and β-sitosterol, were identified by direct analysis of the methanol extract of S. herbacea without pretreatment by GC-MS. Conversely, the analysis of the TMS-derivatized extract revealed 28 distinct peaks. Quantitative analysis further indicated that the predominant compounds in the S. herbacea extract were sugars and sugar derivatives, notably glucose, fructose, and glucitol. The collective concentration of these sugars and its derivatives amounted to 116.45 mg/g, representing 11.6% of the dry weight of the raw S. herbacea. Following sugars and their derivatives, fatty acids constituted the next most abundant group of compounds. However, the presence of amino acids and organic acids was relatively low.

• 대한화장품학회지
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• 제42권1호
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• pp.65-73
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• 2016

대한민국 식품의약품안전처(식약처)는 포름알데하이드 분석법으로 2,4-dinitrophenylhydrazine(DNPH) 유도체화-고성능액체크로마토그래프법(HPLC)을 고시하고 있다. 본 연구는 고시법의 복잡한 시료 전처리 과정을 개선하여 화장품 분석에 편리하게 사용할 수 있는 유도체화법을 개발하고자 수행되었다. 전처리법을 간단하게 하기 위하여 pH, 시간 및 온도 등 반응조건을 최적화하였다. 이 전처리법은 초산염 완충액(pH 5.0)을 사용한 검액의 pH 조정, 디클로로메탄을 사용한 액-액 분획 그리고 감압농축기를 사용한 증발건조와 같이 식약처 고시법의 복잡한 과정이 필요 없다. 유도체화 과정을 통하여 생성된 formaldehyde dinitrophenylhydrazone(formaldehyde-DNP)는 식약처의 시험방법을 약간 변형한 역상 HPLC법으로 분리하고 정량하였다. 2 ~ 40 ppm 농도 범위의 표준액들을 가지고 수행한 검량선 작성 결과, 본 시험법은 상관계수 값이 0.9999로 좋은 직선성을 보여주었다. 본 실험의 최소검출한계(LOD)와 최소정량한계(LOQ)는 각각 0.2 ppm과 0.5 ppm이었다. 또한 회수율 실험결과는 실험방법이 매우 정확하고 재현성이 높음을 보여주었다. 따라서 본 연구에서 제안된 시험법은 화장품 중 포름알데하이드를 신속하게 분석하는데 적용될 수 있을 것이다.

• Bulletin of the Korean Chemical Society
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• 제22권1호
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• pp.9-10
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• 2001

• Archives of Pharmacal Research
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• 제20권5호
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• pp.486-490
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• 1997

A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with (S)-(-)-${\alpha}$-methyl-benzyl isocyanate, the diastereomeric derivatives were resolved $(R_s=1.59)$ on $5{\mu}M$ octadecylsilan column using 47% methanol as a mobile phase with fluorescence detection. The detection limit of each enantiomer was 10 ng/ml (S/N=3).

• Archives of Pharmacal Research
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• 제9권3호
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• pp.131-138
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• 1986

A specific and sensitive gas chromatographic (GC) procedure with the flame photometric detector (FPD) was developed for determination of barbiturates such as barbital, allobarbital, secobarbital, phenobarbital and thiopental in plasma. In order to evaluate the performance of the FPD, the results were campared with those of the flame ionization detector (FID). After extraction of barbiturates from plasma, the barbiturates were quantitatively N, N-dimethylthiometyl (MTM)-derivatized with methylthiomethyl chloride in 1, 8-diazabicyclo [5, 4, 0] undec-7-ene catalyst. The data indicate that the FPD is about 4 times more sensitive than the FID for barbiturates, although it is less reproducible. The FPD also produced chromatogram with less back ground for extracted plasma sample. The FPD also produced chromatogram with less background for extracted plasma sample. The minimum detectable amount of MTM-thiopental on 3% OV-225 column was 4, 4fmol and that of other MTM-barbiturate was about 10.0fmol.

• 분석과학
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• 제6권4호
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• pp.411-415
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• 1993

지방산을 UV 검출기를 사용하여 HPLC로 분석하기 위하여 2-bromoacetyltriphenylene을 유도체화제로 응용하였다. 18-crown-6-ether를 촉매로 한 유도체화반응은 매우 신속, 간편하고 정량적으로 진행되었으며, HPLC상에서 지방산의 검출한계가 1ng 수준으로 그 감도가 양호하였다. 또한 $C_{12}$부터 $C_{22}$까지 9종류의 포화지방산이 역상컬럼상에서 acetonitrile-물 gradient 조건으로 동시에 분리가 가능하였다. 이를 응용하면 각종 생체 시료로부터 미량의 지방산들에 대한 동시분석이 가능하리라 기대된다.

• 약학회지
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• 제59권1호
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• pp.6-11
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• 2015

A simple HPLC-UV method was developed and validated for the quantification of human serum isepamicin using phenylisocyanate as a derivatization agent. The linear calibration curve was obtained in the concentration range of $1{\sim}100{\mu}g/ml$ and LLOQ of $1{\mu}g/ml$. This method was validated with selectivity, linearity, precision and accuracy, leading to successful application for estimating the pharmacokinetic parameters of isepamicin in Korean healthy subjects following IV infusion of 800 mg isepamicin. The mean $t_{1/2}$ of isepamicin was $1.55{\pm}0.08hr$.

• 통합자연과학논문집
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• 제4권3호
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• pp.182-186
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• 2011

Chemical modification of porous silicon surface has been investigated to have different physical surface properties. Porous silicon modified with dodecyl functionality exhibits hydrophobic feature, however the oxidation of porous silicon to modify with hydroxyl group displays hydrophilic properties. Surface characterization for both dodecyl and hydroxyl derivatized porous silicon was investigated by FT-IR spectroscopy. To determine the surface coverage, the amine functionalized surface was reduced by dithiothreitol (DTT) and the released 2-thiopyridone was quantified by UV/vis spectroscopy.