• Title/Summary/Keyword: in situ derivatization

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The preliminary evaluation of semi-quantitative analysis by in situ pre-chromatographic derivatization of amines and image analysis in TLC (TLC상 분리 전 직접적 유도체화 반응과 이미지 분석을 통한 아민 화합물의 반정량분석을 위한 선행평가)

  • Kim, Younsu;Choi, Sung-Woon
    • Analytical Science and Technology
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    • v.28 no.2
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    • pp.79-85
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    • 2015
  • A preliminary experiment was performed to develop a fast, convenient, and economical semi-quantitative method of analyzing amphetamine-like amines from images of derivatives. These were generated from the reaction (in situ, co-spot) of three amphetamine-like compounds with three derivatization reagents on a TLC plate. The attempt was made to optimize the reaction conditions for an efficient derivatization reaction, and TLC images taken by a digital camera were analyzed using two types of image analysis program (CP Atlas 2.0 and ImageJ) for repeatability (RSD, %) and linearity (R2). Then, their results were compared. For efficient derivatization, the reaction conditions needed to be modified. The results of image analysis of each of the samples at two different concentrations (0.5 mg/mL and 0.01 mg/mL) showed that the RSD values for reaction repeatability were in the range of 0.69-5.50%. From the calibration curves between the area of the derivative and the concentration of amines, the R2 values (R2 > 0.9906) for good linear correlation were found to be high, in a concentration range of 0.1-0.005 mg/mL of amines. In addition, the two programs demonstrated little difference in the analysis of repeatability and linearity of the derivatization, so that the current method has the potential to be used for the semi-quantitative analysis of amines.

Immunochemical Determination of Plant Constituents (1990년 제23회 학술발표회 논문초록)

  • 성철기
    • Journal of the Korean Society of Tobacco Science
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    • v.12 no.1
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    • pp.29-38
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    • 1990
  • Until relatively recently plant scientists have made little use of immunological techniques. Now, however, more and more researchers are discovering the powder of these techniques for the screening of immunomodulators and for the detection, quantitative determination and localization of compounds in plant materials. Especially, the recent developments in the fields of plant biotechnology and plant genetic engineering make it even more important for forkers in the plant sciences to become acquainted with the more sophisticated methods. The possible methods include onestep purification of antigens, visualization in situ by immunocytochemis try and on polyacrylam ids gel s by ni trocellulose Western blotting and quantification by various immunoassay. Among them, in this reviews, the quantitative determination methods are to be reviewed. There are several kinds of methods for the quantitative determination of plant constituents such as colorimetry, TLC, GLC, DCC, UV derivatization, densitometry and HPLC. When the complexity of plant constituents is considered. densitometry and HPLC have many advantages in sensitivity and separation ability. After a 11 some advarltages of two methods meritiorled above, all of these methods have many disadvantages and inconveniences. Previous purification for the application of all these methods make them less sensitive and more tedious. Immunoassay can solve these problems in part. But immunoassay also has some limitations. Specificity of immunoassay, contrary, can be considered to be disadvantages. Including this the advantages and disadvantages of immunoassay are to be discussed.

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Enantioselective Preparation of Metoprolol and Its Major Metabolites

  • Jung, Sang-Hun;Linh, Pham-Tuan;Lim, Hee-Kyun;Kim, Hyun-Ju;Kim, Kyeong-Ho;Kang, Jong-Seong
    • Archives of Pharmacal Research
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    • v.23 no.3
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    • pp.226-229
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    • 2000
  • To obtain the standard compounds of metoprolol for a pharmacokinetic study, a convenient synthetic procedure to prepare enantiomers of metoprolol (3a) and its major metaboites, 2-4-(2-hydroxy-3-isopropylamino)propoxyphenylathanol (3b) and 4-(2-hydroxy-3- isopropylamino) pro-poxyphenylacetic acid (4), was developed from their respective starting materials, 4-(2-methoxyethyl)phenol (1a), 4-(2-hydroxyethyl)phenol (1b) and methyl 4-hydroxyphenylacetate (1c). These phenolic compounds (1a, b, c) were converted in situ to their corresponding phenoxides with sodium hydroxide treatment followed by (R)- or (S)-epichlorohydrin treatment. The resulting epoxides 2 were transformed to 3 through reaction with isopropylamine. Ester 3c was hydrolyzed to the metabolite 4. Measured using the HPLC method on chiral column without any derivatization, the optical purity of enantiomers of metoprolol and o-demethylated metabolite 3b ranged between 96-99 % ee and that of enantiomers of carboxylic acid metabolite 4 ranged 91% ee.

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