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1.
Foods ; 13(3)2024 Feb 01.
Article de Anglais | MEDLINE | ID: mdl-38338600

RÉSUMÉ

Sausages are loved by people for their unique texture, satisfying chewiness, and pleasant flavor. However, in the production of sausages, red meat and a large amount of fat are mainly used, and long-term consumption will increase the risk of diseases such as obesity, heart disease, hypertension, and cancer. Our previous studies have shown that the intake of red meat and fat can be reduced through the replacement of lean meat and fat in sausages by Lentinula edodes and Pleaurotus eryngii mushrooms, but this will lead to the deterioration of the gel of sausage products and seriously affect the sensory quality of sausages. In this study, the response surface method was used to optimize the amount of balsa fish skin gelatin, soy protein isolate, and starch added to, and the proportion of Lentinula edodes mushrooms replacing lean meat in, the new sausage, with Pleaurotus eryngii mushrooms replacing fat. The results show that Lentinula edodes mushrooms replaced 36.1% of the lean meat, and the addition of 0.96% balsa fish skin gelatin, 10.61% starch, and 9.94% soy protein isolate resulted in the highest sensory score and the sensory quality being the closest to that of traditional sausages. Compared with the control group, this novel sausage exhibits characteristics such as lower fat and saturated fatty acid content, reduced energy levels, and higher levels of amino acids (aspartic acid, glutamic acid, cysteine, methionine, and proline) and polyunsaturated fatty acids. The total phenolic content of the novel sausage is 12.52 times higher than that of the control. In comparison with the control group, the novel sausage demonstrates a 65.58% increase in DPPH radical scavenging activity and a 3.88-fold improvement in ABTS+ radical scavenging activity. These findings highlight the outstanding antioxidant performance of the novel sausage. This study provides new ideas for improving the sensory quality of new sausages, promoting the healthy development of the sausage industry, and promoting the high-value utilization of edible mushrooms.

2.
IEEE Trans Cybern ; PP2022 Aug 09.
Article de Anglais | MEDLINE | ID: mdl-35943996

RÉSUMÉ

The highly dimensional characteristic of time series brings many challenges on direct mining time series, such as high cost in time and space. Granular computing provides a potential strategy for representing and dealing with time series at a higher level of abstraction. In this study, we propose an information granulation-based weighted fuzzy C-means (wFCM) method to realize time-series clustering, which could avoid high dimensionality processing and provide a concise and visible granular prototype for each cluster. In this method, each time series is first transformed into a series of information granules with trend following the principle of justifiable granularity. The formed granular time series can well capture the main features lying in the original time series and help realize dimensionality reduction. Then, the wFCM method is developed to complete time-series clustering in the granular space. Here, the dynamic time warping (DTW) is extended to capture the similarity for trend-based granular time series. Furthermore, the weighted DTW barycenter averaging is introduced to derive prototypes presented in a granular format, capturing the level, the fluctuation, and the changing trend, which are meaningful and understandable clustering results. The experiments conducted on real-world datasets coming from the UCR time-series database and Chinese stocks are presented to illustrate the effectiveness and practicality of the designed time-series clustering model.

3.
Electrophoresis ; 43(9-10): 1059-1067, 2022 05.
Article de Anglais | MEDLINE | ID: mdl-35362108

RÉSUMÉ

Antibody-based therapeutic proteins have highly complex molecular structures. The final therapeutic protein product may contain a wide range of charge variants. Accurate analysis of this charge variant composition is critical to determine manufacturing process consistency and protein stability and ultimately helps to ensure that patients receive a safe and efficacious product. Here, a highly sialylated bispecific antibody (bsAb-1) challenged the ability to monitor stability by imaged capillary isoelectric focusing (iCIEF). This challenge was overcome by optimization of the iCIEF master mix buffer (adjustment of urea concentration, addition of l-arginine) and enzymatic removal of sialic acid. The method was qualified by assessing linearity, precision, LOD, LOQ, accuracy, and robustness in accordance with ICH guidance. Main species loss detectability increased up to approximately fivefold compared to the iCIEF method without desialylation when monitoring changes in stressed samples. Importantly, the results of the iCIEF method with desialylation correlated with results obtained through LC-MS tryptic peptide mapping and enabled analysis of formulation development stability samples. Finally, this analytical method shows the potential to assess low-concentration formulation development samples down to a sample concentration of 0.1 mg/ml.


Sujet(s)
Électrophorèse capillaire , Acide N-acétyl-neuraminique , Chromatographie en phase liquide , Électrophorèse capillaire/méthodes , Humains , Focalisation isoélectrique/méthodes , Spectrométrie de masse
4.
IEEE Trans Cybern ; 52(9): 9101-9110, 2022 Sep.
Article de Anglais | MEDLINE | ID: mdl-33635821

RÉSUMÉ

Granular computing has been an intense research area over the past two decades, focusing on acquiring, processing, and interpreting information granules. In this study, we focus on the granulation of time series and discover the overall structure of the original time series by clustering the granular time series. During the granulation process, when time series exhibit some trend (up trend, equal trend, or down trend) or consist of a variety of tendencies, the trend is essential to be involved to construct the granular time series. Following the principle of justifiable granularity, we propose to form a series of trend-based information granules to describe the original time series and effectively reduce its dimensionality. Then, the similarity measure between trend-based information granules is provided, and considering the dynamic feature of time-series data, dynamic time warping (DTW) distance is generalized to measure the distance for granular time series. In sum, we show here a novel way of forming trend-based granular time series and the corresponding similarity measure, then based on this, the hierarchical clustering of granular time series is realized. The proposed approach can capture the main essence of time series and help to reduce the computing overhead. Experimental results show that the designed approach can reveal meaningful trend-based information granules, and provide promising clustering results on UCR and real-world datasets.

5.
IEEE Trans Cybern ; 51(12): 6253-6261, 2021 Dec.
Article de Anglais | MEDLINE | ID: mdl-32112690

RÉSUMÉ

In this article, we propose a two-stage time-series clustering approach to cluster time series with different shapes. The first step is to represent the time series by a suite of information granules following the principle of justifiable granularity to perform dimensionality reduction, while the second step is to realize the fuzzy clustering of the time series in the transformed representation space (viz., the space of information granules). In the dimensionality reduction process, the numerical data are granulated using a collection of information granules forming a new sequence that can well describe the original time series. Then, when clustering the time series, dynamic time warping (DTW) is employed to measure the similarity between time series and DTW barycenter averaging (DBA) is generalized to weighted DBA to be involved in the fuzzy C -means (FCMs) algorithm. Finally, the experiments are conducted on the datasets coming from UCR time-series database and Chinese stocks to demonstrate the effectiveness and advantages of the proposed fuzzy clustering approach.


Sujet(s)
Algorithmes , Analyse de regroupements , Bases de données factuelles , Facteurs temps
6.
J Food Sci ; 84(11): 3091-3098, 2019 Nov.
Article de Anglais | MEDLINE | ID: mdl-31627254

RÉSUMÉ

The effects of four treatments of Pleurotus eryngii (king oyster mushroom) as replacements for pork back fat were evaluated for the physicochemical, technological, and sensory properties; nitrite content; and amino acid profile in pork sausages. Five batches were manufactured: one control (formulated with pork back fat) and four treatments with raw, boiled, deep-fried, and fried P. eryngii to replace the pork back fat in sausages. The results indicated that the fat content and energy value decreased, while the protein, moisture, total dietary fiber content, cooking loss, and water-holding capacity of the modified sausages increased. All samples were judged acceptable for their sensory characteristics, with the best one being the sausage containing deep-fried P. eryngii. The raw and fried P. eryngii decreased the residual nitrite content in the sausages. Boiled P. eryngii enhanced the essential amino acids content in the sausages, while the other P. eryngii treatments improved the nonessential amino acid content. In summary, P. eryngii may potentially replace fat in sausages. PRACTICAL APPLICATION: In manufacturing pork sausages, the mushroom P. eryngii can substitute pork back fat to improve the nutritional quality by reducing fat and energy value, while enhancing the protein and total dietary fiber content in the sausages. Raw and fried P. eryngii decreased the residual nitrite content in the sausages. This study provides a basis for preparing healthier alternatives to traditional sausages by substituting pork fat with mushrooms.


Sujet(s)
Matières grasses alimentaires/analyse , Substituts de matières grasses/analyse , Manipulation des aliments/méthodes , Produits carnés/analyse , Pleurotus , Suidae , Acides aminés/analyse , Animaux , Fibre alimentaire/analyse , Pleurotus/composition chimique , Viande rouge/analyse , Goût
7.
Meat Sci ; 156: 44-51, 2019 Oct.
Article de Anglais | MEDLINE | ID: mdl-31125946

RÉSUMÉ

The effects of substituting pork lean meat with Lentinula edodes (LE) on the physicochemical properties, amino acid content, cooking loss, texture, total phenolic content, antioxidant activity, microstructure, microbiological analysis, and sensory characteristics of sausages were evaluated. Five formulations were used in the production of sausages: the control (the pork lean meat formulation) and the four different samples in which LE substituted 25%, 50%, 75%, and 100% of pork lean meat. The results showed that LE improved the moisture, total dietary fiber, methionine, glutamic, cysteine, and total phenolic content; cooking loss; and antioxidant activity of the sausage. By contrast, LE reduced the levels of protein, ash, pH, as well as the energy level and texture of the sausage. No difference was observed between the treatments for fat content, water activity and microorganisms of sausages. In addition, LE led to slight darkening of the sausages. From the sensory point of view, all modified sausages were considered acceptable, and the pork lean meat with 25% substitution by LE exhibited best sensory characteristics. In a word, LE is a promising ingredient to partially replace the lean meat in sausages.


Sujet(s)
Qualité alimentaire , Produits carnés/analyse , Champignons shiitake , Acides aminés/analyse , Animaux , Cuisine (activité) , Fibre alimentaire/analyse , Femelle , Manipulation des aliments/méthodes , Humains , Mâle , Adulte d'âge moyen , Suidae , Goût
8.
Int J Biol Macromol ; 133: 51-57, 2019 Jul 15.
Article de Anglais | MEDLINE | ID: mdl-30981772

RÉSUMÉ

Active films based on chitosan incorporated Herba Lophatheri extract (HLE) with different concentrations were developed. Physicochemical properties of the chitosan films incorporated HLE, including density, opacity, moisture content, color, water solubility, swelling, water vapor permeability and oil resistance were measured. Biological activities of the films include antioxidant activity and antimicrobial properties, which were characterized in terms of 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging activity and Oxford cup method, respectively. The potential interactions between chitosan and HLE in the films were investigated by Attenuated total reflectance-Fourier transform infrared analysis and X-ray diffraction. The results indicated that the moisture content, water solubility, swelling degree, water vapor permeability and oil absorption rate of chitosan/HLE films decreased up to 14.81%, 38.97%, 48.03%, 69.23% and 80% in comparison with the control chitosan film. The DPPH free radical scavenging activity of chitosan/HLE films increased by nearly 3.5 folds, and the diameter of inhibitory zone of the chitosan/HLE films extract solution against Staphylococcus aureus and Escherichia coli increased 17.02% and 19.28%, respectively. Additionally, the incorporation of HLE caused interactions between chitosan and HLE and gave rise to the chitosan/HLE films more opacity, darker, redness and yellowness appearance. In summary, the addition of HLE enhanced the moisture and oil resistance, antioxidant activity which declined with time, and antimicrobial activity of the chitosan film, which were all desirable for food packaging.


Sujet(s)
Phénomènes chimiques , Chitosane/composition chimique , Chitosane/pharmacologie , Extraits de plantes/composition chimique , Poaceae/composition chimique , Antibactériens/composition chimique , Antibactériens/pharmacologie , Dérivés du biphényle/composition chimique , Cadhérines/effets des médicaments et des substances chimiques , Couleur , Piégeurs de radicaux libres/composition chimique , Piégeurs de radicaux libres/pharmacologie , Phénomènes optiques , Perméabilité , Picrates/composition chimique , Solubilité , Staphylococcus aureus/effets des médicaments et des substances chimiques , Vapeur
9.
J Pharm Anal ; 8(5): 324-332, 2018 Oct.
Article de Anglais | MEDLINE | ID: mdl-30345147

RÉSUMÉ

Current trends in chiral analysis of pharmaceutical drugs are focused on faster separations and higher separation efficiencies. Core-shell or superficially porous particles (SPP) based chiral stationary phases (CSPs) provide reduced analysis times while maintaining high column efficiencies and sensitivity. In this study, mobile phase conditions suitable for chiral analyses with electrospray ionization LC-MS were systematically investigated using vancomycin as a representative CSP. The performance of a 2.7 µm SPP based vancomycin CSP (SPP-V) 10 cm × 0.21 cm column was compared to that of a corresponding 5 µm fully porous particles based analogue column. The results demonstrated that the SPP-V column provides higher efficiencies, 2-5 time greater sensitivity and shorter analysis time for a set of 22 basic pharmaceutical drugs. The SPP-V was successfully applied for the analysis of the degradation products of racemic citalopram whose enantiomers could be selectively identified by MS.

10.
J Chromatogr A ; 1443: 93-100, 2016 Apr 22.
Article de Anglais | MEDLINE | ID: mdl-26993781

RÉSUMÉ

A novel method based on high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was developed for the sensitive determination of glyphosate and its major degradation product, AMPA in environmental water samples. The method involves the use of MS compatible mobile phases (0.1% formic acid in water and acetonitrile) for HPLC and direct analysis of water samples without sample derivatization. The method has been validated in different types of water matrices (drinking, surface and groundwater) by accuracy and precision studies with samples spiked at 0.1, 7.5 and 90 ppb. All mean accuracy values ranged from 85% to 112% for glyphosate and AMPA using both primary and secondary quantitative ion transitions (RSD ≤ 10%). Moreover, both primary and secondary ion transitions for glyphosate and AMPA can achieve the quantitation limits at 0.1 ppb. The linear dynamic range of the calibration curves were from 0.1 to 100 ppb for each analyte at each ion transitions with correlation coefficient higher than 0.997.


Sujet(s)
Chromatographie en phase liquide à haute performance , Surveillance de l'environnement/méthodes , Glycine/analogues et dérivés , Phosphonates/analyse , Spectrométrie de masse en tandem , Eau/composition chimique , Glycine/analyse , Isoxazoles , Limite de détection , Tétrazoles ,
11.
Anal Chim Acta ; 912: 74-84, 2016 Mar 17.
Article de Anglais | MEDLINE | ID: mdl-26920775

RÉSUMÉ

It is well-known that matrix effects in high performance liquid chromatography coupled to electrospray ionization mass spectrometry (HPLC-ESI-MS) can seriously compromise quantitative analysis and affect method reproducibility. Paired ion electrospray ionization (PIESI) mass spectrometry is an approach for analyzing ultra-low levels of anions in the positive ion mode. This approach uses a structurally optimized ion pairing reagent to post-column associate with the anionic analyte, subsequently forming positively charged complexes. These newly formed complex ions are often more surface-active as compared to either the native anion or the ion pairing reagent. No studies have examined whether or not the PIESI approach mitigates matrix effects. Consequently, a controlled study was done using five analytes in highly controlled and reproducible synthetic groundwater and urine matrices. In addition, two different mass spectrometers (linear ion trap and triple quadrupole) were used. Compared to the negative ion mode, the PIESI-MS approach was less susceptible to matrix effects when performed on two different MS platforms. Using PIESI-MS, less dilution of the sample is needed to eliminate ionization suppression which, in turn, permits lower limits of detection and quantitation.


Sujet(s)
Anions/analyse , Spectrométrie de masse ESI/méthodes , Chromatographie en phase liquide à haute performance/méthodes
12.
Talanta ; 149: 103-109, 2016.
Article de Anglais | MEDLINE | ID: mdl-26717820

RÉSUMÉ

A sensitive and selective HPLC-MS/MS method was developed for the quantitative analysis of dicamba residues in raw agricultural commodities (RACs). Instead of analysis in the traditionally used negative electrospray ionization (ESI) mode, these anionic compounds were detected in positive ESI with the use of ion-pairing reagents. In this approach, only a small amount (60µM) of a commercially available dicationic ion-pairing reagent was introduced into the post-column sample stream. This method has been validated in six different types of RACs including corn grain, corn stover, cotton seed, soybean, soy forage and orange with satisfactory quantitative accuracy and precision. The limits of quantitation (LOQ) values for these analytes were 1.0 to 3.0µg/kg. The standard curves were linear over the range of the tested concentrations (3.0 to 500µg/kg), with correlation coefficient (r) values≥0.999. Evaluation of ionization effects in RAC matrix extracts using diluent blanks for comparison showed no significant matrix effects were present.


Sujet(s)
Dicamba/analyse , Herbicides/analyse , Résidus de pesticides/analyse , Chromatographie en phase liquide à haute performance , Citrus sinensis , Contamination des aliments/analyse , Fruit/composition chimique , Indicateurs et réactifs/composition chimique , Pyrrolidines/composition chimique , Graines/composition chimique , Glycine max , Spectrométrie de masse ESI , Spectrométrie de masse en tandem , Zea mays
13.
Talanta ; 143: 320-327, 2015 Oct 01.
Article de Anglais | MEDLINE | ID: mdl-26078166

RÉSUMÉ

A new paired ion electrospray ionization tandem mass spectrometry method for determination of anionic surfactants in water samples was developed. In this method, dicationic ion-pairing reagents were complexed with monoanionic analytes to facilitate analyte detection in positive mode electrospray ionization - mass spectrometry. Single ion monitoring and selected reaction monitoring on a triple quadrupole instrument were performed and compared. Four dicationic reagents were tested for the determination of perfluorooctanoic acid (PFOA), perfluorooctane sulfonate (PFOS), sodium dodecyl sulfate (SDS), dodecylbenzene sulfonic acid (DBS), and stearic acid (SA), among other common anions. The obtained limits of detection were compared with those from previous literature. Solid phase extraction using a C18 cartridge was performed in order to eliminate matrix interferences. A literature review was compiled for the methods published between 2010 and 2015 for determination of anionic surfactants. The optimized method was more sensitive than previously developed methods with LOD values of 2.35, 35.4, 37.0, 1.68, and 0.675 pg for SDS, SA, DBS, PFOS, and PFOA, respectively. The developed method was effectively applied for the determination of anionic surfactants in different water samples such as bottled drinking water, cooking water, tap water, and wastewater.


Sujet(s)
Tensioactifs/analyse , Acides alcanesulfoniques/analyse , Benzènesulfonates/analyse , Caprylates/analyse , Eau de boisson/analyse , Fluorocarbones/analyse , Dodécyl-sulfate de sodium/analyse , Spectrométrie de masse ESI , Acides stéariques/analyse , Spectrométrie de masse en tandem , Eaux usées/analyse , Polluants chimiques de l'eau/analyse
14.
Chem Commun (Camb) ; 50(57): 7625-7, 2014 Jul 21.
Article de Anglais | MEDLINE | ID: mdl-24895688

RÉSUMÉ

Molybdenum carbide nanotubes (Mo2C-NTs) were synthesized and showed remarkable catalytic activity for regeneration of an organic sulfide redox shuttle. The dye-sensitized solar cells (DSCs) using Mo2C-NTs as the counter electrode (CE) showed a high power conversion efficiency of 6.22%, which is much higher than the DSCs using a conventional Pt CE (3.91%).

15.
Anal Chem ; 86(5): 2665-72, 2014 Mar 04.
Article de Anglais | MEDLINE | ID: mdl-24506188

RÉSUMÉ

Paired ion electrospray ionization (PIESI) mass spectrometry was developed as a useful technique that provides sensitive detection for anions in the positive ion mode. The ion-pairing reagent (IPR) utilized plays an essential role affecting the detection limits. This work describes the design and synthesis of two novel dications with unsymmetrical structures and their utilization for anion detection and mechanistic insights. The performance of dications was evaluated for seven selected anions in both single ion monitoring (SIM) mode and selected reaction monitoring (SRM) mode. The unsymmetrical dications allowed sensitive detection for these anions with down to subpicogram limits of detection (LOD) and an improved sensitivity from 1.5 to 12 times compared to the corresponding symmetrical dications. The enhanced sensitivity could be attributed to the surface activity of the unsymmetrical dications, which results in a concurrent strong partitioning of the anion to the aerosol droplet surface. Surface activity measurements of the anion/IPR complex were conducted, and a correlation between the observed ESI responses and the surface activity of the complex was found. The mechanism was further explored and explained based on the concepts of the equilibrium partitioning model (EPM).

16.
Sheng Wu Yi Xue Gong Cheng Xue Za Zhi ; 30(3): 552-5, 2013 Jun.
Article de Chinois | MEDLINE | ID: mdl-23865317

RÉSUMÉ

This study was aimed to establish rat bladder tumor animal models to investigate the in viva antitumor effect of polyanhydride-pirarubicin (PAD-THP), a long-lasting anti-cancer implant, in the bladder tumor of animal models. The model of bladder cancer was set up with N-butly-N-(4 hydroxybutyl) nitrosamine (BBN) feeding into rats. The PAD-THP long-acting anti-cancer implants containing the drugs and the same dose of the THP naked drug were placed under the bladder mucosa of bladder tumor model in vivo. The pirarubicin plasma concentration was measured with high performance liquid chromatography (HPLC) detection in vivo. The effective drug concentration and lasting period were observed and compared in the animal bodies. The tumor sizes were measured before and after the treatment. The in viva antitumor effects were analyzed and compared. The results showed that more significant antitumor effect of PAD-THP implants on the local drug release characteristics were presented compared with that of the same dose of THP bare drug group and there were significant differences (P<0. 05) between the two methods. All the results indicated that the PAD-THP anti-cancer implants in the postoperative local treatment of bladder tumors would show prosperous in the future for clinical application.


Sujet(s)
Antinéoplasiques/administration et posologie , Préparations à action retardée/administration et posologie , Implants expérimentaux , Tumeurs de la vessie urinaire/traitement médicamenteux , Animaux , 4-[Butyl(nitroso)amino]butan-1-ol , Modèles animaux de maladie humaine , Doxorubicine/administration et posologie , Doxorubicine/analogues et dérivés , Femelle , Polyanhydrides/administration et posologie , Rats , Rat Sprague-Dawley , Tumeurs de la vessie urinaire/induit chimiquement , Tumeurs de la vessie urinaire/anatomopathologie
17.
J Chromatogr A ; 1223: 47-52, 2012 Feb 03.
Article de Anglais | MEDLINE | ID: mdl-22226552

RÉSUMÉ

A novel type of zwitterionic HILIC stationary phase was prepared by covalently bonding the l-azido lysine on silica gel via click chemistry. The key intermediate azido lysine was synthesized by transformation the amino group in l-Boc-lysine to corresponding azido group and subsequent removal of the N-protected group (Boc). Finally, the azido lysine was covalently bonded to silica beads by click chemistry to get click lysine. Its structure was confirmed by FT-IR and elemental analysis. The new stationary phase showed good HILIC characteristics, when it was applied to separate polar and hydrophilic compounds, such as organic acids, cephalosporins and carbapenems. Compared with the commercial stationary phases, such as Atlantics HILIC and ZIC-HILIC, click lysine displayed better or similar chromatographic behaviors.


Sujet(s)
Azotures/composition chimique , Chromatographie en phase liquide/méthodes , Lysine/analogues et dérivés , Gel de silice/composition chimique , Azotures/synthèse chimique , Chimie click , Interactions hydrophobes et hydrophiles , Lysine/synthèse chimique , Gel de silice/synthèse chimique
18.
Analyst ; 136(24): 5302-7, 2011 Dec 21.
Article de Anglais | MEDLINE | ID: mdl-22025231

RÉSUMÉ

Ion chromatography (IC) is one of the most powerful analysis technologies for the determination of charged compounds. A novel click lysine stationary phase was prepared via Cu(I) catalyzed alkyne-azide 1,3-dipolar cycloaddition (CuAAC) and applied to the analysis of inorganic ions. The chromatographic evaluation demonstrated good performance (e.g. the plate number of thiocyanate is ∼50,000 plates m(-1)) and effective separation ability for the common inorganic anions with aqueous Na(2)SO(4) eluent. The separation mechanism was observed to be mainly dominated by ion exchange interaction. The retention of these analytes is highly dependent on the pH value of eluent. Compared with the lysine stationary phase prepared via the conventional manner, the click lysine exchanger demonstrated shorter retention time and better ion separation characteristics under the same chromatographic conditions, which is a great advantage for rapid separation and analysis of inorganic ions.


Sujet(s)
Chromatographie d'échange d'ions , Lysine/composition chimique , Silice/composition chimique , Alcynes/composition chimique , Anions/composition chimique , Azotures/composition chimique , Catalyse , Chimie click , Cuivre/composition chimique , Humains , Concentration en ions d'hydrogène , Mâle , Nitrates/analyse , Salive/composition chimique
19.
Talanta ; 85(3): 1642-7, 2011 Sep 15.
Article de Anglais | MEDLINE | ID: mdl-21807234

RÉSUMÉ

A novel glycosyl amino acid hydrophilic interaction chromatography (HILIC) stationary phase was prepared via click chemistry. The key intermediate N(3)-glycosyl D-phenylglycine was prepared by a three steps procedure, including selective condensation of amino glucose with N-succinimidyl ester of Boc-D-phenylglycine, deprotection and transformation of amino group to azido group. The structure of all the intermediates and functionalized silica beads were confirmed by (1)H NMR, IR, elemental analysis and (13)C CP-MAS. The chromatography test showed that this new type of separation material possessed good HILIC properties and glycopeptide enrichment characteristics. Nucleosides and bases could be separated in a simple eluent composition (only acetonitrile in combined with water), and with the same condition, these model compounds could not be separated on the commercial HILIC column (Atlantis). Click glycosyl amino acid thus prepared also showed longer retention and better separation ability in the separation of polar organic acids.


Sujet(s)
Acides aminés/composition chimique , Chromatographie en phase liquide à haute performance/instrumentation , Chromatographie en phase liquide à haute performance/méthodes , Glycopeptides/composition chimique , Acétonitriles/composition chimique , Glycopeptides/synthèse chimique , Glycosylation , Humains , Interactions hydrophobes et hydrophiles , Immunoglobuline G/analyse , Immunoglobuline G/composition chimique , Immunoglobuline G/isolement et purification , Modèles chimiques , Structure moléculaire , Nucléosides/analyse , Nucléosides/composition chimique , Nucléosides/isolement et purification , Purines/analyse , Purines/composition chimique , Purines/isolement et purification , Pyrimidines/analyse , Pyrimidines/composition chimique , Pyrimidines/isolement et purification , Reproductibilité des résultats
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