Inherently chiral phosphonatocavitands with various bridging moieties at their wide rim were synthesized. Optical resolution by chiral HPLC was performed with cavitand 8 to afford enantiopure compounds (+)-8 and (-)-8. The molecular structures of hosts 8 and 12 were determined by X-ray diffraction. The host properties were investigated by (1)H and (31)P NMR spectroscopy. The phosphonatocavitand...

A high-performance liquid chromatographic (HPLC) assay suitable for the evaluation of 3-methoxy-4-hydroxyphenylglycol (MHPG) in 1-ml aliquots of plasma is presented. Preparatory steps include extraction into ethyl acetate and minicolumn chromatography. Recoveries are monitored with [3H]MHPG. The HPLC procedure utilizes a C18 column, isocratic elution and amperometric detection. The assay was ch...

Using a ball mill, rapid, atom-economic coupling between adenosine-5'-phosphoromorpholidate and phosphorylated ribose derivatives as their sodium or barium salts was achieved. Facile purification by reversed-phase HPLC enabled product isolation within hours.

The development of glycoanalytical HPLC-based high-throughput technology has greatly enhanced the study of glycobiology, facilitating the discovery of disease-related solutions and providing an informative view of glycosylation and its relationship with other biological disciplines in a systems biology approach.

Various 1,6- and 1,8-naphthalenophanes were synthesized by using the Photo-Dehydro-Diels-Alder (PDDA) reaction of bis-ynones. These compounds are easily accessible from ω-(3-iodophenyl)carboxylic acids in three steps. The obtained naphthalenophanes are axially chiral and the activation barrier for the atropisomerization could be determined in some cases by means of dynamic NMR (DNMR) and/or dyn...

Due to the complex nature of the proteome, instrumentation and methods development for sample cleanup, fractionation, preconcentration, chromatographic separation and detection becomes urgent for the identification of peptides and proteins. Newly developed techniques and equipment for separation and detection, such as nanoHPLC and multidimensional HPLC for protein and peptide separation, enable...

The Commission Decision of EC dated 20 June 2003, on emergency measures concerning hot chilli and hot chilli products coming into any EC member state, required that the consignments of such products should be accompanied by an analytical report showing that they are free of artificial dye Sudan I. The opportunity to set a confirmatory method is evident, and the paper proposes a HPLC/APCI-MS met...

A membrane microcontactor is presented that allows sample pre-treatment by means of extraction and operates in parallel flow mode, hence avoiding an emulsification and compulsory phase separation step. The extraction kinetic behaviour of the device was first evaluated by extraction of a drug candidate, proving equilibrium is reached within 10 min. Next the device was evaluated under more challe...

Dereplication and chemotaxonomic studies of six marine algae of the Ochrophyta and one of the Rhodophyta phyla resulted in the detection of 22 separate compounds. All 16 secondary metabolites, including four new compounds (16-19), could be rapidly dereplicated using HPLC-NMR and HPLC-MS methodologies in conjunction with the MarinLit database. This study highlights the advantages of using NMR da...