Renewable Resources Robert-Jan van Putten,†,‡ Jan C. van der Waal,† Ed de Jong,*,† Carolus B. Rasrendra,‡,⊥ Hero J. Heeres,*,‡ and Johannes G. de Vries* †Avantium Chemicals, Zekeringstraat 29, 1014 BV Amsterdam, the Netherlands ‡Department of Chemical Engineering, University of Groningen, Nijenborgh 4, 9747 AG Groningen, the Netherlands Stratingh Institute for Chemistry, University of Groningen, Nijenborgh 4, 9747 AG Groningen, the Netherlands DSM Innovative Synthesis BV, P.O. Box 18, 6160 MD Geleen, the Netherlands Department of Chemical Engineering, Institut Teknologi Bandung, Ganesha 10, Bandung 40132, Indonesia

Hydroxymethylfurfural, A Versatile Platform Chemical Made from Renewable Resources

5-Hydroxymethylfurfural (HMF) as a building block platform: Biological properties, synthesis and synthetic applications

Some Typical Advances in the Synthetic Applications of Allenes

Separation of polar compounds on polar stationary phases with partly aqueous eluents is by no means a new separation mode in LC. The first HPLC applications were published more than 30 years ago, and were for a long time mostly confined to carbohydrate analysis. In the early 1990s new phases started to emerge, and the practice was given a name, hydrophilic interaction chromatography (HILIC). Although the use of this separation mode has been relatively limited, we have seen a sudden increase in popularity over the last few years, promoted by the need to analyze polar compounds in increasingly complex mixtures. Another reason for the increase in popularity is the widespread use of MS coupled to LC. The partly aqueous eluents high in ACN with a limited need of adding salt is almost ideal for ESI. The applications now encompass most categories of polar compounds, charged as well as uncharged, although HILIC is particularly well suited for solutes lacking charge where coulombic interactions cannot be used to mediate retention. The review attempts to summarize the ongoing discussion on the separation mechanism and gives an overview of the stationary phases used and the applications addressed with this separation mode in LC.

Hydrophilic interaction chromatography.

Hydrophilic interaction liquid chromatography (HILIC) provides an alternative approach to effectively separate small polar compounds on polar stationary phases. The purpose of this work was to review the options for the characterization of HILIC stationary phases and their applications for separations of polar compounds in complex matrices. The characteristics of the hydrophilic stationary phase may affect and in some cases limit the choices of mobile phase composition, ion strength or buffer pH value available, since mechanisms other than hydrophilic partitioning could potentially occur. Enhancing our understanding of retention behavior in HILIC increases the scope of possible applications of liquid chromatography. One interesting option may also be to use HILIC in orthogonal and/or two-dimensional separations. Bioapplications of HILIC systems are also presented.

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Hydrophilic interaction liquid chromatography (HILIC)—a powerful separation technique

Purity testing of organometallic catalysts by packed capillary supercritical fluid chromatography.

Editorial: Multidimensional confusion?

A micro liquid chromatography-mass spectrometry system utilizing 100 μm i. d. packed capillary columns has been used for purity testing of organometallic catalysts. The total effluent, 1 μLmin−1 from the column, was introduced directly into the ion source of a bench-top quadrupole mass spectrometer and electron ionization mass spectra were acquired. In full scan mode a mass limit of detection of 10–15 ng was achieved for the organometallic compounds investigated. The catalysts dimethyl pentamethylcyclopentadienyl iridium dimethylsulphoxide (Cp*Ir(DMSO)Me2) and di(pentamethylcyclopentadienyl dichloro iridium) ((Cp*IrCl2)2) were purity tested and their electron ionization mass spectra recorded. Impurities present down to 1% of the main compound could be determined using large volume injection.

Purity testing of organometallic catalysts by micro liquid chromatography-electron ionization mass spectrometry

A specific, sensitive, and precise assay for simultaneous quantitation of glyceryl trinitrate (GTN) and its metabolites 1,2-and 1,3-glyceryl dinitrate (GDN) has been developed. The method involves one single extraction step with benzene, followed by evaporation at 55°C. One μl of the extract was injected onto a capillary fused silica column with trifluoropropyl as the stationary phase. The column separated all the nitrates within 17 minutes using temperature programming from 90 to 155°C. The lower limits of detection were 0.05, 0.5, and 0.1 nmol/I for GTN, 1,2-GDN and 1,3-GDN respectively. The calibration curves were linear in the concentration ranges 0.05–10.0 nmol/I (GTN), 0.5–10.0 nmol/I (1,2-GDN) and 0.1–10.0 nmol/I (1,3-GDN). Plasma concentration data from two patients receiving intravenous GTN infusion are presented.

Simultaneous determination of glyceryl trinitrate and its metabolites in plasma using capillary gas chromatography with on-column injection

Capillary supercritical fluid chromatography with flame ionization detection has been used to test the purity of air-sensitive organometallic compounds such as bisethenepentamethylcyclopentadienylcobalt (Cp*Co(C2H4)2), dicarbonylcyclopentadienylcobalt (CpCo(CO)2), dicarbonylpentamethylcyclopentadienylcobalt (Cp*Co(CO)2), bisethenepentamethyl cyclopentadienylrhodium (Cp*Rh(C2H4)2), bisethenecyclopentadienylrhodium (CpRh(C2H4)2), carbonyl(1,3-dimesitylimidazol-2-ylidene)cyclopentadienylcobalt (CpCo(CO)(carbene)) and ethene(1,3-dimesitylimidazol-2-ylidene)pentamethylcyclopentadienylrhodium (Cp*Rh(C2H4)(carbene)). A sample introduction cell was constructed for loading of 10–40 mg of the air-sensitive compounds in 100% N2 atmosphere. The sample cell was subsequently filled with toluene or pentane and the analytes in solution were injected onto the 50 μm i.d. capillary column using a timed split injector with 60 nL loop. A nonpolar (5% phenylsiloxane/95% methyl siloxane) stationary phase was used and a mobile phase consisting of 100% CO2 with pressure programming. No signs of air-induced decomposition of the analytes were observed and impurities down to 1% could be determined using SFC-FID. © 2001 John Wiley & Sons, Inc. J Micro Sep 13: 156–162, 2001

Tyge Greibrokk

Papers

Purity testing of organometallic catalysts by packed capillary supercritical fluid chromatography.

Editorial: Multidimensional confusion?

Purity testing of organometallic catalysts by micro liquid chromatography-electron ionization mass spectrometry

Simultaneous determination of glyceryl trinitrate and its metabolites in plasma using capillary gas chromatography with on-column injection

Purity testing of air-sensitive organometallic compounds by capillary supercritical fluid chromatography