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Journal of Separation Science

Yuantao Zhou, Shurui Cao, Cunxian Xi, Jiuyan Chen, Lei Zhang, Xianliang Li, Guomin Wang, Zhiqiong Chen
A magnetic solid-phase extraction adsorbent that consisted of citrus peel-derived nanoporous carbon and silica-coated Fe3 O4 microspheres (C/SiO2 @Fe3 O4 ) was successfully fabricated by co-precipitation. As a modifier for magnetic microspheres, citrus peel-derived nanoporous carbon was not only economical and renewable for its raw material, but exerted enormous nanosized pore structure, which could directly influence the type of adsorbed analytes. The C/SiO2 @Fe3 O4 also possessed the advantages of Fe3 O4 microspheres like superparamagnetism, that could be easily separated magnetically after adsorption...
May 18, 2018: Journal of Separation Science
Dotse Selali Chormey, Süleyman Bodur, Dilgeş Baskın, Merve Fırat, Sezgin Bakırdere
Switchable solvent liquid-phase microextraction was combined with gas chromatography and mass spectrometry to improve the sensitivity and accuracy for the determination of selected endocrine disruptors, pesticides and hormones. The extraction method was used to complement gas chromatography with mass spectrometry by preconcentrating analytes for trace determinations. A Box-Behnken experimental design was used to evaluate the main variables and their interaction effects, and optimum parameters were selected based on the model of experimented results...
May 17, 2018: Journal of Separation Science
Alina Diuzheva, József Balogh, József Jekő, Zoltán Cziáky
A dispersive liquid-liquid microextraction method for the simultaneous determination of 11 pharmaceuticals has been developed. The method is based on a microextraction procedure applied to wastewater samples from different regions of Hungary followed by high performance liquid chromatography with mass spectrometry. The effect of the nature of the extractant, dispersive solvent, different additives and extraction time were examined on the extraction efficiently of the dispersive liquid-liquid microextraction method...
May 17, 2018: Journal of Separation Science
Hongmei Yang, Yihan Wang, Wenjing Yu, Lei Shi, Hongfeng Wang, Rui Su, Changbao Chen, Shuying Liu
The identification and screening of triplex DNA binders are important because these compounds, in many cases, are potential anticancer agents as well as promising drug candidates. Therefore, the ability to screen for these compounds in a high-throughput mode could dramatically improve the drug screening process. A method involving a combination of 96-well plate format and peak area-fading ultra high performance liquid chromatography coupled with Orbitrap mass spectrometry was employed for screening bioactive compounds binding to the triplex DNA from the extracts of Stephania tetrandra S...
May 15, 2018: Journal of Separation Science
Lukáš Taraba, Tomáš Křížek, Petr Kozlík, Ondřej Hodek, Pavel Coufal
Thanks to its high conductivity when acid doped, polyaniline is known as a synthetic metal and is used in a wide range of applications, such as supercapacitors, biosensors, electrochromic devices or solar and fuel cells. Emeraldine is the partly oxidized, stable form of polyaniline, consisting of alternating diaminobenzenoid and iminoquinoid segments. When acidified, the nitrogen atoms of emeraldine become protonated. Due to electrostatic repulsion between positive charges, the polarity and morphology of emeraldine chains presumably change; however, the protonation effects on emeraldine have not yet been clarified...
May 15, 2018: Journal of Separation Science
Ying Zhang, Xiaohu Wu, Tingting Duan, Jun Xu, Fengshou Dong, Xingang Liu, Xiaogang Li, Pengqiang Du, Yongquan Zheng
An ultra high performance liquid chromatography with tandem triple quadrupole mass spectrometry residue method for the quantification and identification of dinotefuran and its main metabolites 1-methyl-3-(tetrahydro-3-furylmethyl) urea and 1-methyl-3-(tetrahydro-3-furylmethyl) guanidine in fruit (watermelon), vegetable (cucumber), cereal (rice), animal-derived foods (milk, egg, and pork), soil and water was developed and validated. The samples were extracted with acetonitrile containing 15% v/v acetic acid and purified with dispersive solid-phase extraction with octadecylsilane, primary secondary amine, graphitized carbon black, or zirconia-coated silica prior to analysis...
May 15, 2018: Journal of Separation Science
Vladimíra Datinská, Karel Klepárník, Barbora Belšánová, Marek Minárik, František Foret
The synthesis and determination of the structure of a Förster resonance energy transfer probe intended for the detection of specific nucleic acid sequences are described here. The probe is based on the hybridization of oligonucleotide modified quantum dots with a fluorescently labeled nucleic acid sample resulting in changes of the fluorescence emission due to the energy transfer effect. The stoichiometry distribution of oligonucleotides conjugated to quantum dots was determined by capillary electrophoresis separation...
May 9, 2018: Journal of Separation Science
Ling Chen, Xueping Dang, Youhong Ai, Huaixia Chen
An acryloyl β-cyclodextrin-silica hybrid monolithic column for pipette tip solid-phase extraction and high-performance liquid chromatography determination of methyl parathion and fenthion have been prepared through a sol-gel polymerization method. The synthesis conditions, including the volume of cross-linker and the ratio of inorganic solution to organic solution, were optimized. The prepared monolithic column was characterized by thermogravimetric analysis, scanning electron microscopy and Fourier transform infrared spectroscopy...
May 7, 2018: Journal of Separation Science
Tamara Alvarez-Segura, J R Torres-Lapasió, María Celia García-Alvarez-Coque
The most efficient optimisation methodologies in liquid chromatography are based on the modelling and prediction of the chromatographic behaviour for each compound in the sample. However, when the column suffers some ageing after the modelling process, predictions may differ significantly from the actual separation. Repeating the modelling is especially troublesome when several columns are involved, as is the case of coupled columns. We propose a shortcut to correct the time and peak profiles in these situations, after evaluating the effects of ageing...
May 6, 2018: Journal of Separation Science
Xiaoying Tang, Xiaoxuan Li, Yuwei Sun, Yin Xiao, Yong Wang
In this work, a novel single sulfoether-bridged cationic per(3,5-dimethyl)phenylcarbamoylated-β-cyclodextrin separation material was prepared by thiol-ene click chemistry and characterized by using FTIR spectroscopy, solid-state 13 C NMR spectroscopy and elemental analysis, which confirmed the correct structure. The separation material exhibited a good achiral separation performance for benzene homologues and phenylamine analogs, especially o-xylene and m-xylene, and m-phenylenediamine and o-phenylenediamine can be discriminated by the (3,5-dimethyl)phenylcarbamoyl cyclodextrins...
May 4, 2018: Journal of Separation Science
Xuehan An, Weibo Chai, Xiaojuan Deng, Hui Chen, Guosheng Ding
In this work, a simple, facile and sensitive magnetic solid-phase extraction method for the extraction and enrichment of three representative steroid hormones before high-performance liquid chromatography analysis was developed. Gold-modified Fe3 O4 nanoparticles, as novel magnetic adsorbents, were prepared by a rapid and environmentally friendly procedure in which polydopamine served as the reductant as well as the stabilizer for the gold nanoparticles, thus successfully avoiding the use of some toxic reagents...
May 2, 2018: Journal of Separation Science
Pamornrat Kueseng, Mudtorlep Nisoa, Chonlatid Sontimuang
The rapid preparation of an atrazine-imprinted polymer in a cost-effective custom-made microwave reactor was demonstrated. The polymerization reaction was accelerated by microwave heating, and the preparation time was greatly shortened (to 1 h). The resulting polymer was successfully applied as solid-phase extraction adsorbent for the selective extraction and preconcentration of atrazine in environmental water samples. The binding capacity of the polymer was 1.11 mg/g polymer. The polymer provided selectivity with higher recovery of atrazine than of other interfering related contaminants...
May 1, 2018: Journal of Separation Science
Micha Tobler, Jitka Caslavska, Patricie Burda, Wolfgang Thormann
High-resolution capillary zone electrophoresis is used to assess the transferrin profile in serum of patients with eight different congenital disorders of glycosylation that represent type I, type II and mixed type I/II disorders. Capillary zone electrophoresis data are compared to patterns obtained by gel isoelectric focusing. The high-resolution capillary zone electrophoresis method is shown to represent an effective tool to assess the diversity of transferrin patterns. Hypoglycosylated disialo-, monosialo- and asialo-transferrin in type I cases can be distinguished from the corresponding underdesialylated transferrin glycoforms present in type II disorders...
April 27, 2018: Journal of Separation Science
Björn Boll, Lena Josse, Anja Heubach, Sophie Hochenauer, Christof Finkler, Jörg Huwyler, Atanas V Koulov
Asymmetric flow field-flow fractionation is a valuable tool for the characterization of protein aggregates in biotechnology owing to its broad size range and unique separation principle. However, in practice asymmetric flow field-flow fractionation is non-trivial to use due to the major deviations from theory and the influence on separation by various factors that are not fully understood. Here we report methods to assess the non-ideal effects that influence asymmetric flow field-flow fractionation separation and for the first time identify experimentally the main factors that impact it...
April 25, 2018: Journal of Separation Science
Weiwei Rong, Sirui Guo, Kewen Ding, Ziyue Yuan, Qing Li, Kaishun Bi
An integrated strategy based on high-resolution mass spectrometry coupled with multiple data mining techniques was developed to screen the metabolites in rat biological fluids after the oral administration of Xanthoceras sorbifolia Bunge husks. Mass defect filtering, product ions filtering and neutral loss filtering were applied to detect metabolites from the complex matrix. As a result, a total of 55 metabolites were tentatively identified, among which, 45 barrigenol type triterpenoids metabolites were detected in the feces, six flavonoids and four coumarins metabolites were in the urine...
April 25, 2018: Journal of Separation Science
Rong Wang, Zilin Chen
A poly(vinylphenylboronic acid-ethylene glycol dimethacrylate) monolithic material incorporated with graphene oxide was synthesized inside a poly(ether ether ketone) tube. This tube with boronate affinity monolith was coupled with a high-performance liquid chromatography system through a six-port valve, and constructed an online solid-phase microextraction with high-performance liquid chromatography system. The performance of this solid phase microextraction with high-performance liquid chromatography system was demonstrated by standard glycoprotein in aqueous samples, namely, horseradish peroxidase...
April 23, 2018: Journal of Separation Science
Akihiro Saito, Mariko Hamano, Hiroyuki Kataoka
This study described an automated on-line method for the simultaneous determination of 8-isoprostane, 8-hydroxy-2'-deoxyguanosine, and 3-nitro-l-tyrosine in human urine. The method involves in-tube solid-phase microextraction using a Carboxen 1006 PLOT capillary column as an extraction device, followed by liquid chromatography with tandem mass spectrometry using a CX column and detection in the negative/positive switching ion-mode by multiple reaction monitoring. Using their stable isotope-labeled internal standards, each of these oxidative stress biomarkers showed good linearity from 0...
April 20, 2018: Journal of Separation Science
Elif Yıldız, Hasan Çabuk
An analytical method is presented for the determination of paraben preservatives in semi-solid cream samples by matrix solid-phase dispersion combined with supramolecular solvent-based microextraction. Due to the oily and sticky nature of the sample matrix, parabens were first extracted from the samples by matrix solid-phase dispersion using silica as sorbent material with a clean-up performed with tetrahydrofuran in the elution step. The eluate (500 μL), 1-decanol (120 μL) and water (4.4 mL) were then mixed in a polyethylene pipette to form supramolecular solvent...
April 20, 2018: Journal of Separation Science
Lizong Chen, Rongyu Wang, Li Cui, Xiao Wang, Leilei Wang, Fanyong Song, Wenhua Ji
Five iridoid glycosides were prepared using molecularly imprinted solid phase extraction combined with preparative high-performance liquid chromatography. Hydrophilic molecularly imprinted polymers were synthesized using α-1-allyl-2-N-acetyl glucosamine, which introduced an abundance of hydrophilic groups into the polymers. Using molecularly imprinted solid-phase extraction as the sample pretreatment procedure, five iridoid glycosides, gardenoside, geniposide, shanzhiside, geniposidic acid, and genipin-1-O-gentiobioside, were selectively enriched from Gardenia fructus extracts...
April 20, 2018: Journal of Separation Science
Dananjaya Kalu Appulage, Evelyn H Wang, Benjamin J Figard, Kevin A Schug
A multipath liquid chromatography with mass spectrometry instrument was constructed with the help of restricted access media to on-line segregate small and large molecules. This liquid chromatography system was custom built with five pumps and three two-position six-port valves to control the flow in a multipath system for the simultaneous analysis of small molecules and proteins. On separate chromatographic channels, small molecules trapped and proteins excluded from the on-line restricted access media were analyzed downstream using high efficiency columns and a triple quadrupole mass spectrometer...
April 20, 2018: Journal of Separation Science
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