Journal of Separation Science

Cover image for Vol. 37 Issue 8

Impact Factor: 2.591

ISI Journal Citation Reports © Ranking: 2012: 25/75 (Chemistry Analytical)

Online ISSN: 1615-9314

HPLC 2012

The HPLC 2012 deals with latest advances achieved in separations carried out in liquid phase, listen to news concerning the related techniques, and get insight into variety of exciting applications using new column technologies, micro- and nanodevices, different -omics, diagnostics and plenty of other interesting information. This virtual online only issue covers recently published papers dealing with liquid chromatography from several separation science journals as e.g. Journal of Separation Science, ELECTROPHORESIS, Mass Spectrometry Reviews, and many more. Treat yourself, read these articles for free and get valuable information.

High-performance liquid chromatographic enantioseparation of amino compounds on newly developed cyclofructan-based chiral stationary phases
Anita Aranyi, Ágnes Bagi, István Ilisz, Zoltán Pataj, Ferenc Fülöp, Daniel W. Armstrong and Antal Péter
Journal of Separation Science
Separation of amino acid amides, amino alcohol, and diamine stereoisomers was performed on recently developed CSPs containing derivatized CF6 and CF7 as chiral selector. It was found that the enantioseparation was enthalpy driven. The elution sequences were determined but no general rule could be established.
Keywords: Analyte structure, Building blocks, Chiral/nonchiral interaction, Stereoisomer
Cited: 1 time
Cited by J. Chromatogr. A

Adsorbents and columns in analytical high-performance liquid chromatography: A perspective with regard to development and understanding
Klaus K. Unger and Athanasios I. Liapis
Journal of Separation Science
This paper represents an attempt to highlight the evolution of adsorbents in the course of HPLC development and tries to diagnose the situation with respect to advancements in material design and adsorbent characterisation and their separation potential in HPLC.
Keywords:Analytical HPLC, Evolution of reversed-phase silica, HETP approach, Modelling approaches, Van Deemter equation

Development of an online capillary comprehensive 2D-LC system for the analysis of proteome samples
Eduardo Sommella, Francesco Cacciola, Paola Donato, Paola Dugo, Pietro Campiglia and Luigi Mondello
Journal of Separation Science
An LC×LC platform for proteomic samples was developed for the first time. Both dimensions were implemented on a capillary column scale thus reducing solvent consumption and boosting sensitivity. Such an approach is promising due to limited quantities of proteomic samples. In addition, MS detection through a Nano-ESI interface will be employed for unequivocal identification of target peptides in biological samples of clinical relevance.
Keywords: Multidimensional LC, Peptide, Stop-flow
Cited: 1 time
Cited by J. Chromatogr. A

Analysis of glycoforms on the glycosylation site and the glycans in monoclonal antibody biopharmaceuticals
Ebru Uçaktürk
Journal of Separation Science
This article tries to show the importance of analytical techniques to monitor glycoforms on the glycosylation site and glycans in mAb drugs. Different modes of chromatographic methods reported in the literature have been explained in detail and some drawbacks and advantages of these methods have been also given. In addition, analytical methods to determine glycoforms on the glycosylation site in mAb drugs have been summarized.
Keywords: Biotechnology, Glycoprotein, Immunoglobulin
Cited: 1 time
Cited by Glycoconjugate J.

Synthesis and bioanalytical evaluation of morphine-3-O-sulfate and morphine-6-O-sulfate in human urine and plasma using LC-MS/MS
Maria Andersson, Tomasz Janosik, Hamid Shirani, Johnny Slätt, Andreas Fischer and Olof Beck
Journal of Separation Science
An LC-MS/MS method for determination and quantification of M3S and M6S in human urine and plasma was developed. The purpose is to apply the method to the study of morphine pain treatment of neonates and for study of abnormal metabolic patterns of heroin addicts. Our study confirms that the morphine sulfate conjugates are less abundant than the glucuronides. For the first time the presence of M3S in urine and plasma as morphine metabolites using highly selective mass spectrometry technique could be demonstrated.
Keywords: Body fluid, Heroin, Metabolite, Morphine, Pain treatment

Retention prediction of a set of amino acids under gradient elution conditions in hydrophilic interaction liquid chromatography
Helen Gika, Georgios Theodoridis, Fulvio Mattivi, Urska Vrhovsek and Adriani Pappa-Louisi
Journal of Separation Science
In the present study, the potential of a retention time prediction algorithm to compute/determine retention of amino acids in HILIC mode was investigated. 21 amino acids were analyzed on a modified silica column under HILIC conditions by ESI-MS/MS. Our results show that the system can provide acceptable retention and chromatographic features for amino acids. This method could have great significance in e.g. metabolomics that rely on HPLC-MS to identify large numbers of compounds.
Keywords: Full scan MS, Linear retention model, Polar metabolite
Cited: 1 time
Cited by Anal. Bioanal. Chem.

Graphene-coated fiber for solid-phase microextraction of triazine herbicides in water samples
Qiuhua Wu, Cheng Feng, Guangying Zhao, Chun Wang and Zhi Wang
Journal of Separation Science
A graphene-coated SPME fiber has been prepared and applied for the extraction of four triazine herbicides (atrazine, prometon, ametryn and prometryn) in water. The extraction efficiencies of the G-coated fiber for the triazine herbicides were much higher than those obtained with two commercial SPME fibers, CW/TPR and PDMS/DVB. This study may serve as a useful guidance for the application of the G-based fibers in the extraction of organic contaminants in water.
Keywords: Carbon material, Environment, Fiber-coating material
Cited: 1 time
Cited by TrAC, Trends Anal. Chem.

Performance of different separation methods interfaced in the same MS-reflection TOF detector: A comparison of performance between CE versus HPLC for biomarker analysis
William Mullen, Amaya Albalat, Julien Gonzalez, Panagiotis Zerefos, Justyna Siwy, Julia Franke and Harald Mischak
No single technique has emerged that can cope with detecting the large number of peptides present and quantifying them over the wide concentration range they exist in. In this investigation, a single (RTOF)-MS analyzer was used to which a CE system and then a nano-flow HPLC was connected. Both techniques showed similar results in terms of number of peptides detected and the mass range the peptides were detected over. The major differences in terms of biomarker research were the ability in CE to calibrate the migration time of the peptides to allow comparison between samples.
Keywords: Bioanaylsis, Peptide, Proteomics, Single detection system

Simultaneous analysis of cocaine and its metabolites in urine by capillary electrophoresis–electrospray mass spectrometry using a pressurized liquid junction nanoflow interface
Věra Hezinová, Zeineb Aturki, Karel Klepárník, Giovanni D'Orazio, František Foret and Salvatore Fanali
The new developed CZE-MS method for simultaneous separation of cocaine, cocaethylene, benzoylecgonine, norcocaine, and ecgonine methyl ester in urine provides: (i) fast and efficient separation combined with the sensitivity and selectivity of MS, (ii) identification and quantitative determination of these compounds without a derivatization process, and (iii) low consumption of solvents and samples.
Keywords: Bioanalysis, Drug screening, Forensic

Comparative proteomic profiling of human lung adenocarcinoma cells (CL 1–0) expressing miR-372
Juo-Hsin Lai, Tzu-Fang She, Yu-Min Juang, Yeou-Guang Tsay, Ay-Huey Huang, Sung-Liang Yu, Jeremy J. W. Chen and Chien-Chen Lai
Lung cancer is a common malignancy and has a poor overall prognosis. A large-scale protein screening study was conducted to better understand the mechanisms by which miR-372 regulates tumor invasiveness. Most of the identified proteins were associated with lung cancer, tumor invasion, and other cancer cell types. The majority of the proteins identified in this study were related to cell cycle progression and cell proliferation.
Keywords: Bioanalysis, Eukaryotic initiation factor 4A-I, Non-small cell lung cancer (NSCLC), Protein, Tumorigenesis

In-depth performance investigation of a nano-LC gradient generator
Antonella Siviero, Manuela Bergna, Giorgio Famiglini, Alessandra Mantegazza, Pierangela Palma and Achille Cappiello
A novel gradient generator for nano-LC has been described here. The point of strength of this gradient generator is the combination of simplicity and robustness. A direct control over the gradient shape can be obtained even at lowest flow rates. A particular attention has been devoted to reduce the consumption of the organic solvents during the LC separation and the column conditioning, for a green chromatography and a more economical use of laboratory resources.
Keywords: Cost savings, Green chemistry, Multi-position valve, Nano-LC-MS

Microfluidic chip-based liquid chromatography coupled to mass spectrometry for determination of small molecules in bioanalytical applications
Shu-Ling Lin, Hsin-Yu Bai, Tzuen-Yeuan Lin and Ming-Ren Fuh
This mini-review focus on the commercial microchips coupled to mass spectrometer with the advantages of reduced sample consumption and enhanced sensitivity for the determination of small molecules in bioanalytical applications. With appropriate sample preparation strategies, the commercial chip based LC-MS systems offer the advantages of reduced sample consumption and enhanced sensitivity for high throughput determination of small molecules in various bioanalytical fields such as pharmaceutical and clinical applications.
Keywords: Bioanalysis, Clnincal application, Pharmaceutical application, Preparation strategy

Measurement of serum lamotrigine by high performance liquid chromatography using a phenyltriazine as internal standard
H. Madhavaram, G. A. Woollard and R. A. F. Couch
Drug Testing and Analysis
It could be shown that irsogladine is a good replacement for BWA725C in the therapeutic drug monitoring of lamotrigine by HPLC, in the likely event that BWA725C is not available. The advantage is that it has a similar phenyltriazine structure to lamotrigine. Further it is not commonly used in human therapeutics, and is therefore an ideal internal standard.
Keywords: Drug monitoring, Irsogladine, Structure similarity

A clinical assay for the measurement of milrinone in plasma by HPLC mass spectrometry
B. Chihoho, A. B. Sage, R. T. Smolenski, A. Vazir, M. L. Rose, N. R. Banner and N. V. Leaver
Biomedical Chromatography
Milrinone is a bipyridine phosphodiesterase inhibitor with positive inotropic and vasodilatory effects. As interest in longer term use of intravenous therapy increases, it becomes essential to monitor its plasma concentration. A complete assay (including sample preparation and analysis) comprising six calibrators, three quality control samples and a single clinical sample could easily be completed within 1 h. This method offers the high specificity and sensitivity of mass spectrometry, is rapid, robust and easy to use and therefore could become the reference procedure for monitoring of milrinone therapy.
Keywords: Heart failure, Therapeutic drug monitoring,

Development and validation of a liquid chromatography/electrospray ionization tandem mass spectrometry method for the quantification of latanoprost free acid in rabbit aqueous humor and ciliary body
Alessio Zammataro, Claudine Civiale, Rosaria Saletti and Salvatore Foti
Journal of Mass Spectrometry
This paper describes the development and validation of a rapid, sensitive, selective and reliable HPLC-MS/MS method to quantify latanoprost free acid in rabbit aqueous humor (AH) and ciliary body. The validated assay offers significant advantages in terms of sensitivity and selectivity, simple sample preparation and fast run time of analysis. After the extraction procedures, the recovery of the analyte is >97% in both matrices, and the matrix effect is 7%. The assay is intended for conventional pre-clinical studies that are necessary for the therapeutical use of the latanoprost formulations.
Keywords: Glaucoma treatment, Intraocular pressure, Prostaglandin F2 alpha
Cited: 1 time
Cited by Eye

Direct-EI in LC–MS: Towards a universal detector for small-molecule applications
Achille Cappiello, Giorgio Famiglini, Pierangela Palma, Elisabetta Pierini, Veronica Termopoli, and Helga Trufelli
Mass Spectrometry Reviews
This review article will give an up-to-date and exhaustive overview on the efficient use of electron ionization (EI) to couple liquid chromatography and mass spectrometry (LC-MS) with an innovative interface called direct-EI. In fact, although atmospheric pressure ionization (API) methodologies have boosted the use of LC-MS, the related analytical methods are sometime affected by inaccurate quantitative results, due to unavoidable and unpredictable ME. The direct-EI interface can represent the basis for a forthcoming universal LC-MS detector for small molecules. Of course, the evolution of the direct-EI-LC-MS interface continues in different directions, including sensitivity, ease-of-use, and new applications.
Keywords: electron ionization, matrix effects, nano-HPLC
Cited: 5 times
Cited by Anal. Bioanal. Chem., Anal. Chem., J. Chromatogr. A, J. Mass Spectrom.

Simultaneous determination of the quantity and isotopic signature of dissolved organic matter from soil water using high-performance liquid chromatography/isotope ratio mass spectrometry
Andrea Scheibe, Lars Krantz and Gerd Gleixner
Rapid Communications in Mass Spectrometry
In recent years a growing interest in the role of dissolved organic matter (DOM) for carbon transport, storage and release in soils, including its sources and fates could be seen. Here, the accuracy and utility of a modified high-performance liquid chromatography/isotope ratio mass spectrometry (HPLC/IRMS) system for measuring the amount and stable carbon isotope signature of dissolved organic matter (DOM) 1 µm was assessed. The method was also applied to natural samples and the concentration and isotopic signature, obtained with HPLC/IRMS, were compared with the results obtained using other techniques.
Keywords: C-13 Aanalysis; Carbon Isotope; Delta-C-13; Dynamics; Forest; Nitrogen; Sugar; Terrestrial ecosystem
Cited: 1 time
Cited by Environ. Sci. Technol.

Resolution of racemic 3-hydroxy-4,5-dimethyl-2(5H)-furanone (sotolon) by packed column supercritical fluid chromatography
Jianchun Xie, Huilan Han, Lei Sun, Huiying Zeng and Baoguo Sun
Flavour and Fragrance Journal
Resolution of racemates using pSFC is a powerful technique for rapid generation of enantiomers. The optimum analytical separation was achieved after the CSP of Chiralpak AD-H. The present work has demonstrated method development and preparative isolation of optically active sotolon from the synthetic molecule of racemic sotolon by the environmentally friendly and rapid approach of pSFC
Keywords: Chiral separation, Enantiomer, 3-Hydroxy-4,5-dimethyl-2-(5H)-furanone, Resolution, Sotolon