• Title/Summary/Keyword: trimethylsilyl

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Protein Hydrolysis with Formic Acid and Analysis of Amino Acid Using Butylthiocarbamyl - trimethylsilyl (BTC - TMS) Derivatives by Gas Chromatography

  • 우강융;이동선;김민철
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.3
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    • pp.320-324
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    • 2003
  • The protein hydrolysis with 6 M formic acid containing 0.3% tryptamine was a superior method for amino acid analysis of standard amino acid and protein than 6 M HCI containing 0.3% tryptamine. The recoveries of standard amino acid after acid hydrolysis were more accurate in the 6 M formic acid hydrolysis than 6 M HCI hydrolysis, especially recovery of tryptophan showed higher values of 1.5 times than that of 6 M HCI hydrolysis. The results of analysis on the standard protein, bovine serum albumin, showed very similar values compared to the sequence analysis reported in the literature for the 6 M formic acid hydrolysis than 6 M HCI hydrolysis, especially in the tryptophan recovery as standard amino acid recovery. Butylthiocarbamyl - trimethylsilyl (BTC - TMS) derivatives of 22 standard amino acids were successfully resolved DB-17 capillary column. Excellent reproducibility of standard amino acid recovery and composition of bovine serum albumin were obtained with BTC-TMS derivatives.

Surface Modification of Ba0.6Sr0.4TiO3 by Trimethylsilyl Chloride as a Silylation Agent (Trimethylsilyl Chloride를 Silylation Agent로 사용한 Ba0.6Sr0.4TiO3 나노입자의 표면개질 연구)

  • Lee, Chan;Han, Wooje;Park, Hyung-Ho
    • Journal of the Microelectronics and Packaging Society
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    • v.26 no.4
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    • pp.127-132
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    • 2019
  • In this study, barium strontium titanate (BSTO) with high dielectric perovskite structure was synthesized by liquid-solid solution synthesis and the surface was modified using trimethylsilyl chloride (TMCS) as a silylation agent. Silylation surface modification is a method of reacting -OH ligand on the surface of BSTO nanoparticles with Cl in TMCS to generate HCl and replacing the ligand on the surface of nanoparticles with -Si, -CH3. Silylation was optimized by varying the concentration of TMCS, and the structure of the silicon network was confirmed by Fourier-transform infrared spectroscopy. In addition, the crystallinity of BSTO nanoparticles was confirmed by X-ray diffractometer and the size of the nanoparticles was calculated using Scherrer equation. The field emission scanning electron microscopic image observed the change of the surface-modified BSTO particle size, and the contact angle measurement confirmed the hydrophobic property of the contact angle of 120.9° in the optimized nanoparticles. Finally, the surface-modified BSTO dispersion experiment in de-ionized water confirmed the hydrophobic degree of the nanoparticles.

Propylene/Nitrogen Separation Membranes Based on Amphiphilic Copolymer Grafted from Poly(1-trimethylsilyl-1-propyne) (양친성 고분자가 그래프팅된 Poly(1-trimethylsilyl-1-propyne) 기반의 프로필렌/질소 분리막)

  • Park, Cheol Hun;Lee, Jae Hun;Park, Min Su;Kim, Jong Hak
    • Membrane Journal
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    • v.29 no.2
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    • pp.88-95
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    • 2019
  • Hydrocarbons containing carbon double bonds are generally called olefins and it is extensively used in petro-chemical industry as essential base material. Especially, olefins are essential in polymer synthesis and thus the effective separation and purification of olefins from gas mixture are very important and it gives significant positive effect on the future industrial development. In this study, we fabricated polymeric composite membrane based on poly(1-trimethylsilyl-1-propyne) (PTMSP) for propylene/nitrogen separation and enhancement of its separation performance by grafting amphiphilic copolymer. Furthermore, to accelerate facilitated transport for propylene molecules, Ag salt ($AgBF_4$) and ionic liquid ($EMIM-BF_4$) was incorporated to polymer composite membranes. The neat PTMSP membrane exhibited extremely high gas permeance and low gas selectivity due to its high free volume. To address this issue, PTMSP was grafted with poly(oxyethylene glycol methacrylate) (POEM) and poly(ethylene glycol) behenyl ether methacrylate (PEGBEM). Additionally, the additives such as $AgBF_4$ and $EMIM-BF_4$ further increased the propylene permeance, resulting in increment of propylene/nitrogen selectivity.

Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA derivative (TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석)

  • Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.107-114
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    • 2006
  • Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

Reactions of Phosphites with Nitroalkene Derivatives: Syntheses of $\beta$-Keto Phosphonates and $\alpha$-Cyanoalkylphosphonates

  • 김대영;오동영
    • Bulletin of the Korean Chemical Society
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    • v.18 no.9
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    • pp.994-998
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    • 1997
  • The addition of phosphite derivatives 1 to nitroalkenes 2 afforded α-phosphoryl nitronates which, on treatment MCPBA, were converted β-keto phosphonates 3. A versatile reaction conditions to generate α-phosphoryl nitronates were examined. α-Cyanoalkylphosphonates 6 were prepared from the diethyl trimethylsilyl phosphite (DTSP) 1c with nitroalkenes 2 and followed by reduction.

Reaction Phosphite with Acetal Derivatives:Syntheses of 1-Alkoxymethylphosphonates and 1-Alkylthiomethylphosphonates

  • 김대영;한동일;오동영
    • Bulletin of the Korean Chemical Society
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    • v.19 no.2
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    • pp.226-230
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    • 1998
  • 1-Alkoxymethylphosphonates 4 and 1-alkylthiomethylphosphonates 5 can be prepared by the reaction of actal derivatives and diethyl trimethylsilyl phosphite in the presence of Lewis acid under mild conditions. The dependency of the chemoselectivities with Lewis acid on the reaction of O,S-acetals with phosphites is described.

Determination of the PDE-5 Inhibitors and Their Analogues by GC-MS and TMS Derivatization

  • Pyo, Jae-Sung;Lee, Hee-Sang;Park, Yu-Jin;Jo, Ji-Yeong;Park, Yong-Hoon;Choe, Sang-Gil;Lee, Mi-Young;Lee, Jae-Sin
    • Mass Spectrometry Letters
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    • v.3 no.1
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    • pp.15-17
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    • 2012
  • Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.