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RISS 인기검색어
- 검색키워드
- 주제어 : Trifluoroacylation (검색결과 4 건)
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윤혜란 대한약학회 2013 Archives of Pharmacal Research Vol.36 No.3
A rapid analytical method was developed toquantify dibasic amino acids (ornithine, lysine and arginine)after two-step derivatization procedure with good sensitivityand specificity on human plasma. If early diagnosis has notbeen made, patients with inborn metabolic disorders such asHHH syndrome, Hyperornithinemia and dibasic aminoaciduriarapidly progress to sudden death, physical defect ormental retardation resulting in storage of the toxic materialinto the brain. Therefore, it is necessary to develop theanalytical method for rapid screening and/or correct confirmationdiagnosis. The formation of trimethylsilyl derivativeof the carboxylic (COO–) functional group wasperformed by adding MSTFA. Five lL of methyl orangewas added to the residue until the color changed into yellow. Consecutively, the trifluoroacyl derivative of the amino(–NH2) functional group was produced by adding MBTFA. Specific ions was chosen for quantification with followingions; m/z 166 and m/z 212 for ornithine, m/z 180 and m/z 395for lysine, and m/z 292 and, m/z 519 for arginine. A calibrationcurve showed a linear relationship for the dibasicamino acids spiked to pooled normal plasma showing R2 of0.9955–0.9979 in the range of 0.1–600 ng investigated. Theutility of the method for screening and diagnosis was demonstratedby recovery 80–125 % and reproducibility withRSD (9–17 %) at low, medium and high concentrationfortified to pooled plasma. Collectively, the present studysuggest that this method could be useful for diagnosis, screening, therapeutic monitoring of metabolic disorders ondietary therapy with excellent sensitivity and rapidity.
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Yoon, Hye-Ran 대한약학회 2007 Archives of Pharmacal Research Vol.30 No.3
A rapid dried-filter paper plasma-spot analytical method was developed to quantify organic acids, amino acids, and glycines simultaneously in a two-step derivatization procedure with good sensitivity and specificity. The new method involves a two-step trimethylsilyl (TMS) -trifluoroacyl (TFA) derivatization procedure using GC-MS/ selective ion monitoring (GC-MS/SIM). The dried mixture of distilled water and methanol. Methyl orange was added to the residue as an indicator. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bis-trifluoroacetam ide were then added and heated to 60${\circ}$C for 10 and f5 min to produce the TMS and TFA derivatives, respectively. Using this method, the silylation of carboxylic functional groups was carried out, which was followed by the trifluoroacyl derivatization of the amino functional group. Thederivatives were anlyzed by GC-MS/SIM . A calibration cure showed a linear relationship for the target compounds between concentrations of 10-500 ng/mL. The limit of detection and quantification on a plasma spot were 10-90 ng/mL (S/N=9) and 80-500 ng/ mL, respectively. The Correlation coefficient ranged from 0.938 and 0.999. When applied to the samples from positive patients, the method clearly differentiated normal subjects from the patients with various metabolic disorders such as PKU, MSUD, OTC and a Propionic Aciduria. The new developed method might be useful for making a rapid, sensitive and simultaneous diagnosis of inherited organic and amino acid disorders. In addition, this method is expected to be an alternative method for screening newborns for metabolic disorders in laboratories where expansive MS/MS is unavailable.
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Hye-Ran Yoon 대한약학회 2007 Archives of Pharmacal Research Vol.30 No.3
A rapid dried-filter paper plasma-spot analytical method was developed to quantify organic acids, amino acids, and glycines simultaneously in a two-step derivatization procedure with good sensitivity and specificity. The new method involves a two-step trimethylsilyl (TMS) - trifluoroacyl (TFA) derivatization procedure using GC-MS/ selective ion monitoring (GC-MS/SIM). The dried-filter paper plasma was fortified with an internal standard (tropate) as well as a standard mixture of distilled water and methanol. Methyl orange was added to the residue as an indicator. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bis-trifluoroacetamide were then added and heated to 60oC for 10 and 15 min to produce the TMS and TFA derivatives, respectively. Using this method, the silylation of carboxylic functional groups was carried out, which was followed by the trifluoroacyl derivatization of the amino functional group. The derivatives were analyzed by GC-MS/SIM. A calibration cure showed a linear relationship for the target compounds between concentrations of 10-500 ng/mL. The limit of detection and quantification on a plasma spot were 10-90 ng/mL (S/N=9) and 80-500 ng/ mL, respectively. The correlation coefficient ranged from 0.938 and 0.999. When applied to the samples from positive patients, the method clearly differentiated normal subjects from the patients with various metabolic disorders such as PKU, MSUD, OTC and a Propionic Aciduria. The new developed method might be useful for making a rapid, sensitive and simultaneous diagnosis of inherited organic and amino acid disorders. In addition, this method is expected to be an alternative method for screening newborns for metabolic disorders in laboratories where expensive MS/MS is unavailable.
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Hye-Ran Yoon,Yong-Wun An 대한약학회 2010 Archives of Pharmacal Research Vol.33 No.2
If early diagnosis is not made, patients with peroxisomal disorders rapidly progress to sudden death, physical defect or mental retardation resulted in storage of the toxic material into the brain. Therefore, it is necessary to develop the analytical method for rapid screening and/or correct confirmation diagnosis. The method utilizes [2H9]pipecolic acid as internal standard. The formation of trimethylsilyl derivative (TMS) of the carboxylic functional group was performed by adding MSTFA. And then 5 μL of methyl orange was added until the color of methyl orange was to yellow. Consecutively, the trifluoroacyl (TFA)-derivative of the -NH functional group was produced by adding MBTFA. GC-MS was set with specific ions (m/z 282, m/z 297) of the TMSTFA derivative of pipecolic acid for selected ion monitoring. The linearity of pipecolic acid in pooled plasma spots showed 0.9999 in the range of 10-150 ng investigated. The precision and accuracy was within S.D. of 5% (RSD, within 5%) for intra-day and inter-day assay. Normal control value has been determined in plasma spots of infant and adults aged 0-30 (including newborn). The utility of the method was demonstrated by quantifying various concentration of fortified pipecolic acid on a filter plasma spot. The new method was simple with just two step derivatisation, time and labor saving without SPE or liquid-liquid extraction, and convenience of delivery owing to the use of filter paper. The described method could be used for routine analysis, monitoring, and clinical diagnostic application of peroxisomal disorders on dietary therapy.
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