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101.
Preconcentration based on paramagnetic microparticles for the separation of sarcosine using hydrophilic interaction liquid chromatography coupled with coulometric detection
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Ondrej Zitka Zbynek Heger Marketa Kominkova Sylvie Skalickova Sona Krizkova Vojtech Adam Rene Kizek 《Journal of separation science》2014,37(5):465-575
Sarcosine has been identified as a potential prostate cancer marker. To provide determination of this compound, a number of methods are developing. In this study, we optimized a method for its separation by hydrophilic interaction LC with electrochemical detection (ED). Due to the fact that mobile phases commonly used for this type of separation altered the LODs measured by electrochemical detectors, we applied postcolumn dosing of buffer suitable for ED. The optimized conditions were mobile phase A acetonitrile, mobile phase B water in the ratio A/B 70:30, with postcolumn addition of mobile phase C (200 mM phosphate buffer pH 9). The optimal mixing ratio was A + B/C 1:1 with a flow rate of 0.80 mL/min (0.40 + 0.40 mL/min) and detection potential of 1000 mV. Due to the optimization of the parameters for effective separation, which had to meet the optimal parameters of ED, we reached a good resolution for separation also with a good LOD (100 nM). In addition, we successfully carried out sarcosine analysis bound on our modified paramagnetic microparticles with the ability to preconcentrate sarcosine isolated from artificial urine. 相似文献
102.
Kahoun D Rezková S Veskrnová K Královský J Holcapek M 《Journal of chromatography. A》2008,1202(1):19-33
The objective of this study was the determination of 25 phenolic compounds in different mead samples (honeywines) using high performance liquid chromatography (HPLC) with coulometric-array detection and in case of hydroxymethylfurfural with UV detection. Our method was optimized in respect to both the separation selectivity of individual phenolic compounds and the maximum sensitivity with the electrochemical detection. The method development included the optimization of mobile phase composition, the pH value, conditions of the gradient elution and the flow rate using a window-diagram approach. The developed method was used for the determination of limits of detection and limits of quantitation for individual compounds. The linearity of calibration curves, accuracy and precision (intra- and inter-day) at three concentration levels (low, middle and high concentration range) were verified. Mead samples were diluted with the mobile phase at 1:1 to 1:50 ratio depending on the concentration and filtered through a PTFE filter without any other sample pre-treatment. Phenolic compounds concentration was determined in 50 real samples of meads and correlated with meads composition and hydroxymethylfurfural concentration. The most frequently occurred compounds were protocatechuic acid and vanillic acid (both of them were present in 98% samples), the least occurred compounds were (+)-catechin (10% samples) and sinapic acid (12% samples). Vanillin and ethylvanillin, which are used as artificial additives for the taste improvement, were found in 60% and 42% samples, respectively. Hydroxymethylfurfural concentration, as an indicator of honey quality, was in the range from 2.47 to 158 mg/L. Our method is applicable for the determination of 25 phenolic compounds in mead, honey and related natural samples. 相似文献
103.
Tryptophan in Multicomponent Petasis Reactions for Peptide Stapling and Late-Stage Functionalisation
Dr. Sona Krajcovicova Prof. David R. Spring 《Angewandte Chemie (International ed. in English)》2023,62(34):e202307782
Peptide stapling is a robust strategy for generating enzymatically stable, macrocyclic peptides. The incorporation of biologically relevant tags (such as cell-penetrating motifs or fluorescent dyes) into peptides, while preserving their binding interactions and enhancing their stability, is highly sought after. Despite the unique opportunities offered by tryptophan‘s indole scaffold for targeted functionalisation, its utilisation in peptide stapling has been limited as compared to other amino acids. Herein, we present an approach for peptide stapling using the tryptophan-mediated Petasis reaction. This method enables the synthesis of both stapled and labelled peptides and is applicable to both solution and solid-phase synthesis. Importantly, the use of the Petasis reaction in combination with tryptophan facilitates the formation of stapled peptides in a straightforward, multicomponent fashion, while circumventing the formation of undesired by-products. Furthermore, this approach allows for efficient and diverse late-stage peptide modifications, thereby enabling rapid production of numerous conjugates for biological and medicinal applications. 相似文献
104.
A new anthracene glycoside, asperflavin ribofuranoside (1), and the previously described polyketides, flavoglaucin (2), isodihydroauroglaucin (3), and citrinin (4) have been isolated from the marine-derived fungus Microsporum sp. The structure and absolute stereochemistry of a new compound (1) was assigned on the basis of physicochemical data. Compounds 1-3 exhibited a significant radical scavenging activity against 1,1-diphenyl-2-picrylhydrazyl (DPPH) with IC(50) values of 14.2, 11.3, and 11.5 microM, respectively, which are more potent than the positive control, ascorbic acid (IC(50), 20 microM). Compound 1 also showed a moderate antibacterial activity against the methicillin-resistant and multidrug-resistant Staphylococcus aureus (MRSA and MDRSA) with MIC value of 50 microg/ml. 相似文献
105.
Andersen KK Andersen SL Esberg J Knudsen H Mikkelsen R Uggerhøj UI Sona P Mangiarotti A Ketel TJ Ballestrero S;CERN NA 《Physical review letters》2012,108(7):071802
We report the first observation of a shoulder in the radiation spectrum from GeV electrons in a structured target consisting of two thin and closely spaced foils. The position of the shoulder depends on the target spacing and is directly connected to the finite formation length of a low-energy photon emitted by an ultrarelativistic electron. With the present setup it is possible to control the separation of the foils on a μm scale and hence measure interference effects caused by the macroscopic dimensions of the formation length. Several theoretical groups have predicted this effect using different methods. Our observations have a preference for the modified theory by Blankenbecler but disagree with the results of Baier and Katkov. 相似文献
106.
Amin Owais Sinha Subhojyoti Maji Partha Sona Mukherjee Rupam 《Journal of Solid State Electrochemistry》2023,27(9):2387-2394
Journal of Solid State Electrochemistry - We report the effect of indium doping on thermal stability and ionic conductivity of beta alumina NaInxAl11-xO17 solid electrolyte which is synthesized by... 相似文献