Just Published: Journal of Chromatography A

A new issue of this journal has just been published. To see abstracts of the papers it contains (with links through to the full papers) click here:

Journal of Chromatography A

http://rss.sciencedirect.com/publication/science/5248

Selected papers from the latest issue:

2.

An in situ benzoylation-dispersive liquid–liquid microextraction method based on solidification of floating organic droplets for determination of biogenic amines by liquid chromatography–ultraviolet analysis   Original Research Article Pages 1-10 Shaodong Jia, Yeonsuk Ryu, Sung Won Kwon, Jeongmi Lee Highlights ►In situbenzoylation was combined with DLLME-SFO for LC–UV analysis of 9 BAs. ► A simple, green method using a basic LC–UV system was developed. ► The LOD was comparable to or lower than methods using FL or MS detection. ► The versatile method was applied to BA analysis in 4 types of alcoholic beverages.

3.

Multiclass mycotoxin analysis in Silybum marianum by ultra high performance liquid chromatography–tandem mass spectrometry using a procedure based on QuEChERS and dispersive liquid–liquid microextraction   Original Research Article Pages 11-19 Natalia Arroyo-Manzanares, Ana M. García-Campaña, Laura Gámiz-Gracia Highlights ► A UHPLC–MS/MS method is proposed for determination of 15 mycotoxins in milk thistle. ► Sample treatment is based on QuEChERS extraction and DLLME clean-up. ► LOQs are below maximum limits allowed by EU in foods and botanicals. ► RSDs were <10% and recoveries were >60%, except for ZON in seed and CIT in extract. ► The method could be good alternative for multi-mycotoxin determination in botanicals.

4.

Dispersive liquid–liquid microextraction for the determination of macrocyclic lactones in milk by liquid chromatography with diode array detection and atmospheric pressure chemical ionization ion-trap tandem mass spectrometry   Original Research Article Pages 20-26 Natalia Campillo, Pilar Viñas, Gema Férez-Melgarejo, Manuel Hernández-Córdoba Highlights ► Five endectocides are determined in milk samples using liquid chromatography. ► A high sensitivity is achieved due to dispersive liquid–liquid microextraction. ► The procedure allows the EU regulations to be attained using diode array detection.

5.

Purification of lignans from Schisandra chinensis fruit by using column fractionation and supercritical antisolvent precipitation   Original Research Article Pages 27-37 Tai-Ling Huang, Justin Chun-Te Lin, Charng-Cherng Chyau, Kuo-Li Lin, Chieh-Ming J. Chang Highlights ► Using ultrasonic extraction (UE), column fractionation (CF), supercritical anti-solvent (SAS). ► Optimizing operation parameters of UE, CF and SAS were discussed. ► Evaluating economical and environmental aspects for the purification.

Column Liquid Chromatography

6.

Polyphenolic characterization and chromatographic methods for fast assessment of culinary Salvia species from South East Europe   Original Research Article Pages 38-45 I. Cvetkovikj, G. Stefkov, J. Acevska, J. Petreska Stanoeva, M. Karapandzova, M. Stefova, A. Dimitrovska, S. Kulevanova Highlights ► HPLC–DAD–ESI-MSnmethods for characterization of polyphenols in Sage were developed. ► Various extractions were performed and evaluated for their effectiveness. ► The selectivity of different RP C18 stationary phases for polyphenols was evaluated. ► Polyphenolic profile of 118 different Salvia samples was done. ► 68 populations of wildSalviafrom South East Europe were examined.

7.

Effect of the ionic strength on the adsorption process of an ionic surfactant onto a C18-bonded charged surface hybrid stationary phase at low pH   Original Research Article Pages 46-57 Fabrice Gritti, Georges Guiochon Highlights ► Nortriptylinium adsorption behavior on CSH-C18is studied at various pH and ionic strengths. ► Overloaded band profiles recorded and derived from several isotherm models are compared. ► At low loading factors, electrostatic repulsion of ions by the surface affects this behavior. ► At high loading factors the ions are mostly adsorbed as neutral species. ► At high loading factors, a Langmuir–Moreau isotherm best accounts for adsorption behavior.

8.

Adsorption behaviors of neutral and ionizable compounds on hybrid stationary phases in the absence (BEH-C18) and the presence (CSH-C18) of immobile surface charges   Original Research Article Pages 58-71 Fabrice Gritti, Georges Guiochon Highlights ► The adsorption behavior of caffeine and nortriptyline was studied on two RPLC/hybrid phases. ► The bands were eluted with a low ionic strength buffer. ► The band profiles of these compounds were recorded under overloaded conditions. ► The adsorption isotherms and band profiles on both columns are accounted for suitable models. ► The results inform on electrostatic repulsion influence on retention of ionizable compounds.

9.

Screening of the most relevant parameters for method development in ultra-high performance hydrophilic interaction chromatography   Original Research Article Pages 72-83 Aurélie Periat, Benjamin Debrus, Serge Rudaz, Davy Guillarme Highlights ► A dataset of 82 drugs presenting very diverse physico-chemical properties was investigated. ► Five different polar stationary phases packed with sub-2μm particles were tested. ► The Agilent Zorbax RRHD was the most versatile HILIC column packed with sub-2μm particles. ► The nature of the stationary phase and mobile phase pH are the most important parameters for HILIC method development. ► Screening four different stationary phases and two pH appear to be the best initial step for successful HILIC method development.

10.

Scalable Technology for the Extraction of Pharmaceutics: Outcomes from a 3 year collaborative industry/academia research programme   Original Research Article Pages 84-94 Ian Sutherland, Chris Thickitt, Nathalie Douillet, Keith Freebairn, David Johns, Clive Mountain, Philip Wood, Neil Edwards, David Rooke, Guy Harris, David Keay, Ben Mathews, Roland Brown, Ian Garrard, Peter Hewitson, Svetlana Ignatova Highlights ► Collaborative end-user driven study between industry, a supply company and academia. ► Highlights of a comprehensive applications portfolio with 4 detailed case studies. ► Lower solvent usage when compared to solid phase chromatography. ► Projected cost analysis for process scale – material costs significantly lower than for solid phase chromatography.

11.

Layer-by-layer assembly of polyelectrolyte and graphene oxide for open-tubular capillary electrochromatography   Original Research Article Pages 95-101 Qishu Qu, Chenhao Gu, Zuli Gu, Yuqi Shen, Chengyin Wang, Xiaoya Hu Highlights ► Capillary column was coated with GO using PDDA as coupling agent. ► The coating was stable and showed long lifespan. ► Graphene oxide coating was used as stationary phase for CEC separation. ► Various types of compounds including proteins were separated on GO coated column.

12.

On-line study of flavonoids of Trollius chinensis Bunge binding to DNA with ethidium bromide using a novel combination of chromatographic, mass spectrometric and fluorescence techniques   Original Research Article Pages 102-112 Zhiling Song, Hong Wang, Biao Ren, Baobao Zhang, Yuki Hashi, Shizhong Chen Highlights ► Developed a novel online analytical method HPLC-DAD-ESI-IT-TOF-MSnDNA–EB-FLD. ► Identified 18 constituents and six were first found inTrollius chinensisBunge. ► 16 constituents accounted for binding to DNA. ► Correlate chemical profile with DNA activity without isolation and purification.

13.

Effect of the pH and the ionic strength on overloaded band profiles of weak bases onto neutral and charged surface hybrid stationary phases in reversed-phase liquid chromatography   Original Research Article Pages 113-126 Fabrice Gritti, Georges Guiochon Highlights ► The adsorption behavior of weak bases on BEH-C18is heterogeneous at all pH. ► The EML model accounts poorly for changes in this behavior at increasing ionic strength. ► The adsorption behavior of weak bases on CSH-C18is heterogeneous at pH>5. ► This behavior is practically homogeneous at pH<3.

14.

Void exclusion of antibodies by grafted-ligand porous particle anion exchangers   Original Research Article Pages 127-132 Rui Nian, Cindy Chuah, Jeremy Lee, Hui Theng Gan, Sarah Maria Abdul Latiff, Wan Yee Lee, Vincent Vagenende, Yuan-Sheng Yang, Pete Gagnon Highlights ► A new variant of anion exchange chromatography is described. ► IgG is excluded to the void volume from pH 3–10 and 0–4M NaCl. ► Exclusion depends on a variable size exclusion effect mediated by grafted ligands. ► Most host cell proteins follow typical pH and salt trends for anion exchange. ► Greater than 99% reduction of all major contaminants is achieved in a single step.

15.

Speciation of arsenic in marine food (Anemonia sulcata) by liquid chromatography coupled to inductively coupled plasma mass spectrometry and organic mass spectrometry   Original Research Article Pages 133-141 M. Contreras-Acuña, T. García-Barrera, M.A. García-Sevillano, J.L. Gómez-Ariza Highlights ► Focused microwave extraction combined with HPLC–ICP-MS/MS is a powerful approach for arsenic speciation in seafood. ► Glyceryl phosphorylarsenocholine has been reported for the first time in a natural sample. ► Dimethylarsinothioic acid (DMAS) has been reported for the first time in seafood. ► After cooking, 64% of the total arsenic is lost. The dominant species are: DMA>AB>DMAS>AsC>AsV>TETRA>GPAsC>MA>TMAO.

16.

Characterization and quantification of racemic and meso-ethylenediamine-N,N′-bis(2-hydroxy-5-sulfophenylacetic) acid/iron (III) by ion-pair ultra-high performance liquid chromatography coupled with diode array detector and electrospray tandem mass spectrometry   Original Research Article Pages 142-152 Alessandro Biasone, Giusto Cianci, Donata Di Tommaso, Alberto Piaggesi, Emilio Tagliavini, Paola Galletti, Fabio Moretti Highlights ► Synthesis and quantification of EDDHSA ligand. ► Set up of the UHPLC–Vis–ESI/MS method forracandmeso-EDDHSA/Fe determination. ► the stereochemistries of the two EDDHSA/Fe isomers were assigned. ► Mass fragmentation patterns ofracandmeso-EDDHSA/Fe were determined. ► New insights on ion-pair chromatography were provided.

Electrophoresis and Electrochromatography

17.

Determination of biapenem in a medicinal product by micellar electrokinetic chromatography with sweeping in an enhanced electric field   Original Research Article Pages 153-160 Katarzyna Michalska, Judyta Cielecka-Piontek, Genowefa Pajchel, Stefan Tyski Highlights ► MEKC with sweeping in an enhanced electric field enabled effective assay of biapenem. ► The proposed MEKC method is selective, linear, precise and accurate. ► The results obtained by HPLC and MEKC prove that the method is selective. ► It is possible to distinguish particular degradation products. ► The method can be applied as an alternative method for drug analysis control.

18.

Highly sensitive immunoassay of carcinoembryonic antigen by capillary electrophoresis with gold nanoparticles amplified chemiluminescence detection   Original Research Article Pages 161-166 Jing Jiang, Shulin Zhao, Yong Huang, Guoxin Qin, Fanggui Ye Highlights ► A novel capillary electrophoresis noncompetitive immunoassay was proposed. ► The assay was based on AuNPs amplified CL detection to enhance sensitivity. ► This protocol provides a new method for the detection of carcinoembryonic antigen. ► The method showed high sensitivity, selectivity and good repeatability.

Short Communications

Column Liquid Chromatography

19.

Facile optimization for chromatographic separation of liquiritin and liquiritigenin    Pages 167-171 Shaoyan Wang, Min Guo, Jingxiang Cong, Shoujiang Li Highlights ► Liquiritin and liquiritigenin in flavonoids were separated by chromatography. ► Their chromatographic behaviors were described by the linear ED model. ► Chromatographic separation conditions were optimized by simulated calculation. ► The overload and complete separation was realized.

Column Liquid Chromatography, and Electrophoresis and Electrochromatography

20.

Evaluation and comparison of various separation techniques for the analysis of closely-related compounds of pharmaceutical interest    Pages 172-177 Charlotte Gourmel, Alexandre Grand-Guillaume Perrenoud, Laura Waller, Emilie Reginato, Joelle Verne, Bertrand Dulery, Jean-Luc Veuthey, Serge Rudaz, Julie Schappler, Davy Guillarme Highlights ► Various separation techniques were compared for the analysis of closely-related compounds. ► Capillary electrophoresis provided excellent results for basic compounds but generic conditions were not reached. ► Supercritical fluid chromatography was more generic and particularly adapted for neutral and acidic compounds. ► Reversed-phase LC was the most versatile strategy for any class of compounds. ► The selectivity achieved with the three separation techniques was found complementary.

Gas Chromatography

21.

Direct liquid deposition calibration method for trace cyclotrimethylenetrinitramine using thermal desorption instrumentation    Pages 178-182 Christopher R. Field, Adam L. Lubrano, Duane A. Rogers, Braden C. Giordano, Greg E. Collins Highlights ► Cryo-focusing improves reproducibility for liquid and vapor samples. ► Losses are observed using a commercial thermal desorption unit. ► Calibration curves are established using direct liquid deposition of RDX. ► Calibration curves can be established simultaneously for TNT and RDX.

22.

Selective extraction of halogenated compounds from data measured by comprehensive multidimensional gas chromatography/high resolution time-of-flight mass spectrometry for non-target analysis of environmental and biological samples    Pages 183-189 Shunji Hashimoto, Yasuyuki Zushi, Akihiro Fushimi, Yoshikatsu Takazawa, Kiyoshi Tanabe, Yasuyuki Shibata Highlights ► We developed a software finding organo-chlorines or bromines from netCDF mass data. ► We achieved to extracted organo-chlorines or bromines from data of GC×GC–HRTOFMS. ► For accurate data extraction, high mass resolution was essential. ► A mass defect filter was very effective in removing mass spectra of hydrocarbons. ► Direct measurement and data extraction were effective for non-target analysis.

23.

Impurity analyses of high-purity carbon monoxide gas using micro gas chromatography for development as a certified reference material    Pages 190-193 Nobuhiro Matsumoto, Takuro Watanabe, Kenji Kato Highlights ► We analyzed impurities in a high-purity carbon monoxide gas of semiconductor grade. ► A compact micro gas chromatograph was used for the impurity analyses. ► High-accuracy calibration gas mixtures by gravimetric blending method were used. ► The concentration of helium was found to be much higher than the other impurities. ► The purity of the high-purity gas was around 99.996% based on our analyses.

24.

The use of a custom mode electron capture detector to determine mixing ratios of environmental tracers: Sulfur hexafluoride, chlorotrifluoromethane and bromotrifluoromethane    Pages 194-198 J. Rosiek, J. Bartyzel, K. Rozanski, I. Sliwka Highlights ► Resonance mode of ECD operation was optimized for detection of CF3Cl and CF3Br. ► 50-fold amplification of the ECD signal was obtained for CF3Cl. ► 3.5-fold amplification of the ECD signal was obtained for CF3Br. ► Activation energies of CF3Cl and CF3Br were determined.