- In-situ and one-step preparation of protein film in capillary column for open tubular capillary electrochromatography enantioseparation
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In this work, the phase-transitioned BSA (PTB) film using the mild and fast fabrication process adhered to the capillary inner wall uniformly, and the fabricated PTB film-coated capillary column was applied to realize open tubular capillary electrochromatography (OT-CEC) enantioseparation. The enantioseparation ability of PTB film-coated capillary was evaluated with eight pairs of chiral analytes including drugs and neurotransmitters, all achieving good resolution and symmetrical peak shape. For three consecutive runs, the relative standard deviations (RSD) of migration time for intra-day, inter-day, and column-to-column repeatability were in the range of 0.3%–3.5%, 0.2%–4.9% and 2.1%–7.7%, respectively. Moreover, the PTB film-coated capillary column ran continuously over 300 times with high separation efficiency. Therefore, the coating method based on BSA self-assembly supramolecular film can be extended to the preparation of other proteinaceous capillary columns.
- Li, Ling,Xue, Xuqi,Zhang, Huige,Lv, Wenjuan,Qi, Shengda,Du, Hongying,Manyande, Anne,Chen, Hongli
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supporting information
p. 2139 - 2142
(2021/04/07)
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- Method for asymmetrically synthesizing norepinephrine bitartrate
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The invention discloses a preparation method for asymmetrically synthesizing norepinephrine bitartrate. The method is characterized by comprising the following steps: by using chloroacetyl catechol asa raw material, asymmetrically reducing carbonyl in the chloroacetyl catechol into hydroxyl, reacting with urotropine, hydrolyzing with hydrochloric acid to obtain R-norepinephrine, salifying rnorepinephrine and Ltartaric acid are salified to obtain norepinephrine bitartrate, wherein the total yield is larger than or equal to 86%, the ee value is larger than or equal to 95%, and the purity is larger than or equal to 99.6%. The method overcomes the defects in the prior art, and has the advantages that asymmetric reduction is adopted, so that the yield of norepinephrine bitartrate is increased,three wastes and the cost are reduced, and the method is suitable for industrial production.
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- Method for synthesizing noradrenaline
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The invention discloses a method for synthesizing noradrenaline. The method comprises the steps that (-)-diisopinocampheyl chloroborane serves as a catalyst, a reducing agent is utilized in an ether solvent at a low temperature, particularly (-)-diisopinocampheyl chloroborane directly reduces noradrenaline to generate levarterenol, and a solution containing noradrenaline is obtained. According tothe method, levarterenol can be directly obtained by using (-)-diisopinocampheyl chloroborane as the reducing agent, resolution is not needed, and the cost and potential safety hazards are reduced simultaneously.
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Paragraph 0037; 0045; 0046; 0049; 0052; 0057; 0062
(2018/06/04)
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- A Method for Synthesizing a Catecholamine Using Plasma Polymerization
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The present invention relates to a method for manufacturing a catecholamine-based compound using a plasma polymerization method and, more specifically, to a method for artificially synthesizing a unimolecular compound capable of having various catecholamines, i.e. a hydroxyl group (-OH) as a ortho-group of a benzene ring and various alkylamines as a para-group, from a catecholamine precursor material such as phenol, aniline, etc, using a dry plasma polymerization method.COPYRIGHT KIPO 2015
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Page/Page column 19
(2017/01/02)
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- Synthesis of aromatic 1,2-amino alcohols utilizing a bienzymatic dynamic kinetic asymmetric transformation
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The applicability of the recent published bienzymatic protocol for the synthesis of (R)-2-amino-1-phenylethanol was tested using L-threonine aldolase from Pseudomonas putida and L-tyrosine decarboxylase from either Enterococcus faecalis (Efa) or two genes from Enterococcus faecium (Efil, Efi2). In all 21 benzaldehyde derivatives were applied for an initial TLC screening. On a small scale, octopamine and noradrenaline were obtained as (S)-enantiomers using Efil. Three protocols were upscaled yielding enantioenriched (S)-octopamine (yield 99%, ee 81%), (R)-2-amino-1-phenylethanol (yield 61%, ee 62%) and (S)-noradrenaline (yield 76%, ee 79%).
- Steinreiber, Johannes,Schuermann, Martin,Van Assema, Friso,Wolberg, Michael,Fesko, Kateryna,Reisinger, Christoph,Mink, Daniel,Griengl, Herfried
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p. 1379 - 1386
(2008/04/03)
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- Process of protecting a 1,2-aminoalcohol for reductive amination coupling
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A process of protecting a 1,2- or 1,3-aminoalcohol for reductive amination coupling is provided. The alcohol is protected with trimethylsilyl chloride. Trimethylsilyl protected norepinephrine derivatives useful in the preparation of arbutamine are also provided.
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- Pharmaceutical formula
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The present invention concerns a pharmacological vehicle or carrier system, which makes possible administration of the active ingredient with a high absorption thereof in the blood circulation of the patient treated therewith, in particular also in the case of oral administration. The pharmacological vehicle system according to the invention comprises ultrafine particles of a reaction product of a reactive derivative of an at least dibasic inorganic acid or an alkane-carboxylic acid having 2 or 3 carboxyl groups and optionally one or two hydroxy groups, wherein one bond of the dibasic inorganic acid or one carboxy group of the alkane-carboxylic acid is bonded to a pharmacological active ingredient containing a hydroxy group, SH group and/or a primary or secondary amino group having a ractive hydrogen atom on this group, and the other bond is bonded to the free hydroxy group of a glycerolipid having at least one free hydroxy group on the glycerol. The invention further concerns these reaction products and a process for the preparation of ultrafine particles of these reaction products.
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- Ligand Exchange Chromatography of Amino Alcohols. Use of Schiff Bases in Enantiomer Resolution
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A new method for enantiomeric resolution of primary amino alcohols by HPLC is described involving derivatization to the salicylaldehyde Schiff base followed by ligand exchange chromatography (LEC) with chiral L-proline-bonded stationary phases.All of the α-amino alcohols with a hydroxyl substituent on the asymmetric carbon examined were resolved, including catecholamines and other β-hydroxyphenethylamines.The copper(II) ion employed in LEC serves to stabilize the Schiff base, whereas the derivative permits complexation in a manner favorable for resolution and enhanced detection.A possible structure for the mixed complex responsible for separation is suggested.From this structure, a correlation between elution order and configuration is proposed.
- Gelber, Loren R.,Karger, Barry L.,Neumeyer, John L.,Feibush, Binyamin
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p. 7729 - 7734
(2007/10/02)
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