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Chromatography, Volume 2, Issue 1 (March 2015), Pages 1-140

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Editorial

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Open AccessEditorial Acknowledgement to Reviewers of Chromatography in 2014
Chromatography 2015, 2(1), 19; doi:10.3390/chromatography2010019
Received: 9 January 2015 / Accepted: 9 January 2015 / Published: 9 January 2015
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Abstract
The editors of Chromatography would like to express their sincere gratitude to the following reviewers for assessing manuscripts in 2014:[...] Full article

Research

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Open AccessArticle Quantification of Carbonyl Compounds Generated from Ozone-Based Food Colorants Decomposition Using On-Fiber Derivatization-SPME-GC-MS
Chromatography 2015, 2(1), 1-18; doi:10.3390/chromatography2010001
Received: 3 December 2014 / Accepted: 19 December 2014 / Published: 24 December 2014
Cited by 2 | PDF Full-text (1108 KB) | HTML Full-text | XML Full-text
Abstract
Fruit leathers (FLs) production produces some not-to-specification material, which contains valuable ingredients like fruit pulp, sugars and acidulates. Recovery of FL for product recycling requires decolorization. In earlier research, we proved the efficiency of an ozone-based decolorization process; however, it produces carbonyls as
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Fruit leathers (FLs) production produces some not-to-specification material, which contains valuable ingredients like fruit pulp, sugars and acidulates. Recovery of FL for product recycling requires decolorization. In earlier research, we proved the efficiency of an ozone-based decolorization process; however, it produces carbonyls as major byproducts, which could be of concern. A headspace solid-phase microextraction with on-fiber derivatization followed by gas chromatography-mass spectrometry was developed for 10 carbonyls analysis in ozonated FL solution/suspension. Effects of dopant concentration, derivatization temperature and time were studied. The adapted method was used to analyze ozonated FL solution/suspension samples. Dopant concentration and derivatization temperature were optimized to 17 mg/mL and 60 °C, respectively. Competitive extraction was studied, and 5 s extraction time was used to avoid non-linear derivatization of 2-furfural. The detection limits (LODs) for target carbonyls ranged from 0.016 and 0.030 µg/L. A much lower LOD (0.016 ppb) for 2-furfural was achieved compared with 6 and 35 ppb in previous studies. Analysis results confirmed the robustness of the adapted method for quantification of carbonyls in recycled process water treated with ozone-based decolorization. Ethanal, hexanal, 2-furfural, and benzaldehyde were identified as byproducts of known toxicity but all found below levels for concern. Full article
(This article belongs to the Special Issue Solid Phase Micro-Extraction)
Open AccessArticle Determination of Trichloroethylene in Water by Liquid–Liquid Microextraction Assisted Solid Phase Microextraction
Chromatography 2015, 2(1), 66-78; doi:10.3390/chromatography2010066
Received: 12 December 2014 / Accepted: 3 February 2015 / Published: 9 February 2015
Cited by 1 | PDF Full-text (1034 KB) | HTML Full-text | XML Full-text
Abstract
A method for the determination of trichloroethylene (TCE) in water using portable gas chromatography/mass spectrometry (GC/MS) was developed. A novel sample preparation method, liquid–liquid microextraction assisted solid phase microextraction (LLME–SPME), is introduced. In this method, 20 µL of hexane was added to 10
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A method for the determination of trichloroethylene (TCE) in water using portable gas chromatography/mass spectrometry (GC/MS) was developed. A novel sample preparation method, liquid–liquid microextraction assisted solid phase microextraction (LLME–SPME), is introduced. In this method, 20 µL of hexane was added to 10 mL of TCE contaminated aqueous samples to assist headspace SPME. The extraction efficiency of SPME was significantly improved with the addition of minute amounts of organic solvents (i.e., 20 µL hexane). The absolute recoveries of TCE at different concentrations were increased from 11%–17% for the samples extracted by SPME to 29%–41% for the samples extracted by LLME–SPME. The method was demonstrated to be linear from 10 to 1000 ng mL−1 for TCE in water. The improvements on extraction efficiencies were also observed for toluene and 1, 2, 4-trichlorobenzene in water by using LLME–SPME method. The LLME–SPME method was optimized by using response surface modeling (RSM). Full article
(This article belongs to the Special Issue Solid Phase Micro-Extraction)
Open AccessArticle Multivariate DoE Optimization of Asymmetric Flow Field Flow Fractionation Coupled to Quantitative LC-MS/MS for Analysis of Lipoprotein Subclasses
Chromatography 2015, 2(1), 96-117; doi:10.3390/chromatography2010096
Received: 12 December 2014 / Revised: 21 January 2015 / Accepted: 11 February 2015 / Published: 26 February 2015
Cited by 5 | PDF Full-text (3327 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
In this report we demonstrate a practical multivariate design of experiment (DoE) approach for asymmetric flow field-flow fractionation (AF4) method optimization using separation of lipoprotein subclasses as an example. First, with the aid of commercially available software, we built a full factorial screening
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In this report we demonstrate a practical multivariate design of experiment (DoE) approach for asymmetric flow field-flow fractionation (AF4) method optimization using separation of lipoprotein subclasses as an example. First, with the aid of commercially available software, we built a full factorial screening design where the theoretical outcomes were calculated by applying established formulas that govern AF4 channel performance for a 5–35 nm particle size range of interest for lipid particles. Second, using the desirable ranges of instrumental parameters established from theoretical optimization, we performed fractional factorial DoE for AF4 separation of pure albumin and ferritin with UV detection to narrow the range of instrumental parameters and allow optimum size resolution while minimizing losses from membrane immobilization. Third, the optimal range of conditions were tested using response surface DoE for sub-fractionation of high and low density lipoproteins (HDL and LDL) in human serum, where the recovery of the analytes were monitored by fraction collection and isotope-dilution LC-MS/MS analysis of each individual fraction for cholesterol and apolipoproteins (ApoA-1 and ApoB-100). Our results show that DoE is an effective tool in combining AF4 theoretical knowledge and experimental data in finding the most optimal set of AF4 instrumental parameters for quantitative coupling with LC-MS/MS measurements. Full article
(This article belongs to the Special Issue Advances in Hyphenated Methods in Separation)
Figures

Open AccessArticle Analysis of Bioactive Components of Oilseed Cakes by High-Performance Thin-Layer Chromatography-(Bio)assay Combined with Mass Spectrometry
Chromatography 2015, 2(1), 125-140; doi:10.3390/chromatography2010125
Received: 31 December 2014 / Accepted: 9 March 2015 / Published: 17 March 2015
Cited by 3 | PDF Full-text (2435 KB) | HTML Full-text | XML Full-text
Abstract
Hemp, flax and canola seed cakes are byproducts of the plant oil extraction industry that have not received much attention in terms of their potential use for human food instead of animal feed. Thus, the bioactivity profiling of these oilseed cakes is of
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Hemp, flax and canola seed cakes are byproducts of the plant oil extraction industry that have not received much attention in terms of their potential use for human food instead of animal feed. Thus, the bioactivity profiling of these oilseed cakes is of interest. For their effect-directed analysis, planar chromatography was combined with several (bio)assays, namely 2,2-diphenyl-1-picrylhydrazyl scavenging, acetylcholine esterase inhibition, planar yeast estrogen screen, antimicrobial Bacillus subtilis and Aliivibrio fischeri assays. The streamlined high-performance thin-layer chromatography (HPTLC)-bioassay method allowed the discovery of previously unknown bioactive compounds present in these oilseed cake extracts. In contrast to target analysis, the direct link to the effective compounds allowed comprehensive information with regard to selected effects. HPTLC-electrospray ionization-mass spectrometry via the elution-head based TLC-MS Interface was used for a first characterization of the unknown effective compounds. The demonstrated bioactivity profiling on the feed/food intake side may guide the isolation of active compounds for production of functional food or for justified motivation of functional feed/food supplements. Full article
(This article belongs to the Special Issue New Trends in Thin-Layer Chromatography)

Review

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Open AccessReview Development of Monolithic Column Materials for the Separation and Analysis of Glycans
Chromatography 2015, 2(1), 20-65; doi:10.3390/chromatography2010020
Received: 30 November 2014 / Accepted: 28 January 2015 / Published: 9 February 2015
Cited by 5 | PDF Full-text (4254 KB) | HTML Full-text | XML Full-text
Abstract
Monolithic column materials offer great advantages as chromatographic media in bioseparations and as solid-supports in biocatalysis. These single-piece porous materials have an interconnected ligament structure that limits the void volume inside the column, thus increasing the efficiency without sacrificing the permeability. The preparation
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Monolithic column materials offer great advantages as chromatographic media in bioseparations and as solid-supports in biocatalysis. These single-piece porous materials have an interconnected ligament structure that limits the void volume inside the column, thus increasing the efficiency without sacrificing the permeability. The preparation of monolithic materials is easy, reproducible and has available a wide range of chemistries to utilize. Complex, heterogeneous and isobaric glycan structures require preparation methods that may include glycan release, separation and enrichment prior to a comprehensive and site-specific glycosylation analysis. Monolithic column materials aid that demand, as shown by the results reported by the research works presented in this review. These works include selective capture of glycans and glycoproteins via their interactions with lectins, boronic acids, hydrophobic, and hydrophilic/polar functional groups on monolith surfaces. It also includes immobilization of enzymes trypsin and PNGase F on monoliths to digest and deglycosylate glycoproteins and glycopeptides, respectively. The use of monolithic capillary columns for glycan separations through nano-liquid chromatography (nano-LC) and capillary electrochromatography (CEC) and coupling these columns to MS instruments to create multidimensional systems show the potential in the development of miniaturized, high-throughput and automated systems of glycan separation and analysis. Full article
(This article belongs to the Special Issue Monolithic Columns in Separation Sciences)
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Open AccessReview Recent Advances and Uses of Monolithic Columns for the Analysis of Residues and Contaminants in Food
Chromatography 2015, 2(1), 79-95; doi:10.3390/chromatography2010079
Received: 1 January 2015 / Accepted: 4 February 2015 / Published: 10 February 2015
Cited by 4 | PDF Full-text (696 KB) | HTML Full-text | XML Full-text
Abstract
Monolithic columns are gaining interest as excellent substitutes to conventional particle-packed columns. These columns show higher permeability and lower flow resistance than conventional liquid chromatography columns, providing high-throughput performance, resolution and separation in short run times. Monoliths possess also great potential for the
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Monolithic columns are gaining interest as excellent substitutes to conventional particle-packed columns. These columns show higher permeability and lower flow resistance than conventional liquid chromatography columns, providing high-throughput performance, resolution and separation in short run times. Monoliths possess also great potential for the clean-up and preparation of complex mixtures. In situ polymerization inside appropriate supports allows the development of several microextraction formats, such as in-tube solid-phase and pipette tip-based extractions. These techniques using porous monoliths offer several advantages, including miniaturization and on-line coupling with analytical instruments. Additionally, monoliths are ideal support media for imprinting template-specific sites, resulting in the so-called molecularly-imprinted monoliths, with ultra-high selectivity. In this review, time-saving LC columns and preparative applications applied to the analysis of residues and contaminants in food in 2010–2014 are described, focusing on recent improvements in design and with emphasis in automated on-line systems and innovative materials and formats. Full article
(This article belongs to the Special Issue Monolithic Columns in Separation Sciences)
Open AccessReview Recent High Performance Thin Layer Chromatographic Studies on Biomphalaria glabrata (Gastropoda)
Chromatography 2015, 2(1), 118-124; doi:10.3390/chromatography2010118
Received: 9 February 2015 / Revised: 3 March 2015 / Accepted: 5 March 2015 / Published: 10 March 2015
PDF Full-text (633 KB) | HTML Full-text | XML Full-text
Abstract
This review examines the recent high performance thin layer chromatography (HPTLC) literature on the effects of biotic and abiotic factors on certain analytes in the medically important freshwater snail, Biomphalaria glabrata. The analytes studied were lipids, lipophilic pigments, amino acids, and carbohydrates.
[...] Read more.
This review examines the recent high performance thin layer chromatography (HPTLC) literature on the effects of biotic and abiotic factors on certain analytes in the medically important freshwater snail, Biomphalaria glabrata. The analytes studied were lipids, lipophilic pigments, amino acids, and carbohydrates. As determined by HPTLC, various factors, such as larval parasitism, estivation, temperature changes, and others, alter the metabolism of the snail and cause significant changes in the chemical contents of the analytes under study. Full article
(This article belongs to the Special Issue New Trends in Thin-Layer Chromatography)

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