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Journal of Chromatography. A

Siti Baidurah, Paramasivam Murugan, Lee Joyyi, Junya Fukuda, Masaya Yamada, Kumar Sudesh, Yasuyuki Ishida
Thermally assisted hydrolysis and methylation-gas chromatography (THM-GC) in the presence of an organic alkali was validated for the compositional analysis of poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) [P(3HB-co-3HHx)] accumulated in whole bacterial cells. Recombinant Cupriavidus necator Re2058/pCB113 was grown in a batch fermentation with different concentration of palm oil and fructose in order to control the molar fraction of 3HHx in P(3HB-co-3HHx) produced in the cells. Trace amounts (30μg) of freeze-dried cells were directly subjected to THM-GC in the presence of tetramethylammonium hydroxide (TMAH) at 400°C...
October 14, 2016: Journal of Chromatography. A
Artak E Kostanyan
The closed-loop recycling counter-current chromatography (CLR CCC) is performed in several consecutive separation stages. First, the loop is opened, and within a specified time the solution of solutes in the mobile phase is continuously fed to the column. After the solutes loading is finished, the loop is closed, and the first separation stage starts. After a certain number of cycles the first fraction of solutes is eluted, the loop is closed, and the second separation stage starts, and so on. In this study, simple equations are presented allowing the simulation of such separation processes...
October 14, 2016: Journal of Chromatography. A
Fengli Chen, Qiang Zhang, Huiyan Gu, Lei Yang
In this study, a novel approach involving homogenate-circulating ultrasound in combination with aqueous enzymatic extraction (H-CUAEE) was developed for extraction of kernel oil from Pinus pumila. Following comparison of enzyme types and concentrations, an enzyme mixture consisting of cellulase, pectinase and hemicellulase (1:1:1, w/w/w) at a concentration of 2.5% was selected and applied for effective oil extraction and release. Several variables potentially influencing extraction yields, namely, homogenization time, incubation temperature, incubation time, mark-space ratio of ultrasound irradiation, ultrasound irradiation power, liquid-solid ratio, pH and stirring rate, were optimized by Plackett-Burman design...
October 14, 2016: Journal of Chromatography. A
Shanshan Wang, Chao Han, Sisi Wang, Lijuan Bai, Shanshan Li, Jianguang Luo, Lingyi Kong
Cu(II) complexed amino acid ionic liquid, Cu(II)-[1-butyl-3-methylimidazolium][L-Pro] (Cu(II)-[BMIm][L-Pro]), was successfully adopted as chiral ligand to improve the enantioseparation efficiency in high speed counter-current chromatography (HSCCC). For the enantioseparation of intractable naringenin (NRG) racemic mixtures, Cu(II)-[BMIm][L-Pro] coupled with hydroxypropyl-β-cyclodextrin (HP-β-CD) was successfully applied as dual chiral selectors in HSCCC. The influence of important parameters, including the concentration of the chiral selectors, the pH value, and the temperature were investigated...
October 14, 2016: Journal of Chromatography. A
Salvatore Fanali
This paper presents the state of the art concerning the separation of chiral compounds by means of nano-liquid chromatography (nano-LC). The enantiomers' separation and determination are a subject of fundamental importance in various application fields such as pharmaceutical industry, biomedicine, food, agrochemical etc. Nano-LC is a miniaturized chromatographic technique offering some advantages over conventional ones such as low consumption of mobile phase, sample volume and amount of chiral stationary phase, reduced costs etc...
October 14, 2016: Journal of Chromatography. A
Liu Yang, Jie Zhang, Faqiong Zhao, Baizhao Zeng
In this work, a novel poly(3,4-ethylenedioxythiophene)@Au nanoparticles (PEDOT@AuNPs) hybrid coating was prepared and characterized. Firstly, the monomer 3,4-ethylenedioxythiophene was self-assembled on AuNPs, and then electropolymerization was performed on a stainless steel wire by cyclic voltammetry. The obtained PEDOT@AuNPs coating was rough and showed cauliflower-like micro-structure with thickness of ∼40μm. It displayed high thermal stability (up to 330°C) and mechanical stability and could be used for at least 160 times of solid phase microextraction (SPME) without decrease of extraction performance...
October 14, 2016: Journal of Chromatography. A
Rushd Khalaf, Bertrand Coquebert de Neuville, Massimo Morbidelli
Ion exchange chromatography materials functionalized with polyelectrolyte brushes (PEB) are becoming an integral part of many protein purification steps. Adsorption onto these materials is different than that onto traditional materials, due to the 3D partitioning of proteins into the polyelectrolyte brushes. Despite this mechanistic difference, many works have described the chromatographic behavior of proteins on polyelectrolyte brush type ion exchangers with much of the same methods as used for traditional materials...
October 13, 2016: Journal of Chromatography. A
Ji Ye Lee, Na Hyun Park, Wonwoong Lee, Eun Hye Kim, Young Ho Jin, Eun Kyung Seo, Jongki Hong
A comprehensive profiling method was established for the determination of various chemicals in Pinellia (P.) ternata and pedatisecta species. The profiling method comprises a fast ultrasonic extraction with various solvents, followed by GC-MS and LC-APCI-MS analysis. A total of 73 polar components as trimethylsilyl (TMS) derivatives were detected in methanol extract by GC-MS. The main components of the P. species were profiled as several kinds of fatty acids, amino acids, nucleic acids, carbohydrates, and phenolic compounds...
October 13, 2016: Journal of Chromatography. A
Hongjun Xia, Guangping Wan, Junlong Zhao, Jiawei Liu, Quan Bai
High performance liquid chromatography (HPLC) is a kind of efficient separation technology and has been used widely in many fields. Micro-sized porous silica microspheres as the most popular matrix have been used for fast separation and analysis in HPLC. In this paper, the monodisperse large-porous silica microspheres with controllable size and structure were successfully synthesized with polymer microspheres as the templates and characterized. First, the poly(glycidyl methacrylate-co-ethyleneglycol dimethacrylate) microspheres (PGMA-EDMA) were functionalized with tetraethylenepentamine (TEPA) to generate amino groups which act as a catalyst in hydrolysis of tetraethyl orthosilicate (TEOS) to form Si-containing low molecular weight species...
October 13, 2016: Journal of Chromatography. A
Jingqian Xie, Lu Zhao, Kai Liu, Fangjie Guo, Weiping Liu
The chirality of herbicides has been the focus of research. However, there is little information on the enantioseparation of amide herbicides with different chiral elements. In this study, the need for different chiral stationary phases (CSPs), mobile phases, temperatures and flow rates for the separation of napropamide, acetochlor and propisochlor was discussed in detail and compared to metolachlor. Resolution of C-chiral enantiomers was easier than that of axial-chiral enantiomers. Metolachlor and acetochlor could achieve baseline separation only on AY-H and AS-H columns, respectively...
October 13, 2016: Journal of Chromatography. A
Catia Contado, Roberto Argazzi, Vincenzo Amendola
Many advanced industrial and biomedical applications that use silver nanoparticles (AgNPs), require that particles are not only nano-sized, but also well dispersed, not aggregated and not agglomerated. This study presents two methods able to give rapidly sizes of monodispersed AgNPs suspensions in the dimensional range of 20-100nm. The first method, based on the application of Mie's theory, determines the particle sizes from the values of the surface plasmon resonance wavelength (SPRMAX), read from the optical absorption spectra, recorded between 190nm and 800nm...
October 13, 2016: Journal of Chromatography. A
Huazi Wang, Lu Hu, Wanzhen Li, Runhua Lu, Sanbing Zhang, Wenfeng Zhou, Haixiang Gao
A pretreatment method using in-syringe dispersive liquid-liquid microextraction based on the direct solidification of ionic liquids before high performance liquid chromatography analysis was developed for the determination of benzoylurea insecticides (BUs) in honey samples. The hydrophobic ionic liquid [N4444][PF6], formed in situ by the hydrophilic ionic liquid [N4444]Cl and the ion exchange reagent KPF6, was used to extract the target analytes. The entire extraction procedure was performed in a syringe. The extractant was solidified at room temperature and collected using a nylon membrane filter...
October 13, 2016: Journal of Chromatography. A
Alistair K Brown, Charles S Wong
Recent data suggests there are non-trivial amounts of human pharmaceutical conjugates potentially entering environmental surface waters. These compounds could contribute to eliciting toxic effects on aquatic biota either directly or indirectly, via de-conjugation. The need for developing a single method for quantifying both parents and conjugates is necessary. Propranolol (PRO), sulfamethoxazole (SMX), and their respective major conjugates 4-OH-propranolol sulfate (PRO-Sul) and sulfamethoxazole-β-glucuronide (SMX-Glc) were successfully simultaneously extracted through weak anion exchange solid phase extraction cartridges from primary and secondary clarification wastewaters from the North End Winnipeg Water Pollution Treatment Plant in Winnipeg, Canada...
October 11, 2016: Journal of Chromatography. A
Jing Chen, Sudhirkumar Shinde, Prabal Subedi, Celina Wierzbicka, Börje Sellergren, Stefan Helling, Katrin Marcus
Selective enrichment techniques are essential for mapping of protein posttranslational modifications (PTMs). Phosphorylation is one of the PTMs which continues to be associated with significant analytical challenges. Particularly problematic are tyrosine-phosphorylated peptides (pY-peptides) resulting from tryptic digestion which commonly escape current chemo- or immuno- affinity enrichments and hence remain undetected. We here report on significant improvements in this regard using pY selective molecularly imprinted polymers (pY-MIPs)...
October 11, 2016: Journal of Chromatography. A
Mónica Díaz-Bao, Patricia Regal, Rocío Barreiro, Cristina A Fente, Alberto Cepeda
A fast and facile method for the fabrication of magnetic molecularly imprinted stir-bars (MMIP-SB) has been developed, using a combination of imprinting technology and magnetite. Magnetite was prepared in the laboratory from the raw and embedded into molecularly imprinted polymers through a process of bulk polymerization. This novel design was applied to the analysis of aflatoxins, one of the most important groups of mycotoxins in terms of occurrence and toxicity. In the context of food safety, molecularly imprinted polymers are a promising tool to achieve selective and accessible methods of extraction for different residues and contaminants...
October 11, 2016: Journal of Chromatography. A
Ji-Yeon Song, Kyung-Min Kim, Chang-Ha Lee
In this study, a novel operating strategy was developed to improve the separation performance of simulated moving bed (SMB) chromatography by the simultaneous control of product outlet streams and feed inlet stream (SimCon). The SimCon operation can achieve a high separation performance without exceeding the maximum allowable pressure drop in an SMB system. The SimCon operation consisted of three steps within a single switching period: the initial, middle, and last steps. The extract port and feed-inlet port were closed at the initial step, but the raffinate port was closed at the last step...
October 11, 2016: Journal of Chromatography. A
Fabrício de Oliveira Ferreira, Caio Rodrigues-Silva, Susanne Rath
Avermectins and milbemycin are widely used as veterinary drugs and as agricultural pesticides, and their residues have been detected in soil. This study reports a simple and high-throughput method for determining ivermectin (IVER), abamectin (ABA), doramectin (DORA), eprinomectin (EPRI), and moxidectin (MOXI) residues in soils, employing an on-line solid-phase extraction technique coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (SPE-UHPLC-MS/MS). The method was validated and applied for the determination of ABA in soils from an orange plantation treated with this pesticide...
October 11, 2016: Journal of Chromatography. A
J T Oberlerchner, P Vejdovszky, T Zweckmair, A Kindler, S Koch, T Rosenau, A Potthast
Degraded celluloses are becoming increasingly important as part of product streams coming from various biorefinery scenarios. Analysis of the molar mass distribution of such fractions is a challenge, since neither established methods for mono- or disaccharides nor common methods for polysaccharide characterization cover the intermediate oligomer range appropriately. Size exclusion chromatography (SEC) with multi-angle laser light scattering (MALLS), the standard approach for celluloses, suffers from decreased scattering intensities in the lower-molar mass range...
October 8, 2016: Journal of Chromatography. A
A S Uzhel, A V Zatirakha, O I Shchukina, A D Smolenkov, O A Shpigun
A number of covalently-bonded hyperbranched poly(styrene-divinylbenzene)-based (PS-DVB) anion exchangers having functional ion exchange layers of different branching degrees are prepared and investigated. The attachment of the hyperbranched functional layers to the substrate surface is realized via anchor secondary amino groups inserted into the polymeric backbone by means of acylation with acetic anhydride followed by reductive amination with methylamine. Further modification of the obtained secondary amino groups is provided by repeating the steps of alkylation with 1,4-butanediol diglycidyl ether (1,4-BDDGE) and amination of the terminal epoxide rings with methylamine (MA)...
October 7, 2016: Journal of Chromatography. A
N Rodríguez-González, E Beceiro-González, M J González-Castro, M F Alpendurada
A fast, simple, selective and sensitive method has been developed for the determination of nine triazine herbicides (ametryn, atrazine, cyanazine, prometryn, propazine, simazine, simetryn, terbuthylazine and terbutryn) and eight degradation products (desethyl atrazine, desethyl-desisopropyl atrazine, desethyl 2-hydroxyatrazine, desethyl terbuthylazine, desisopropyl atrazine, desisopropyl 2-hydroxyatrazine, 2-hydroxyatrazine and 2-hidroxyterbuthylazine) in seawater samples. On-line solid-phase extraction coupled with ultra-pressure liquid chromatography-tandem mass spectrometry was employed for simultaneous analysis of all compounds in 11min...
October 6, 2016: Journal of Chromatography. A
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