[Dietary supplements on the domestic market adulterated with sildenafil and tadalafil].

Mandatory requirements regulating the manufacture and sale of dietary supplements are much less stringent than those related to pharmaceuticals. Hence, the sheer number and diversity of marketed products in this category has shown an unprecedented increase Europe-wide. Not surprising, that cases for incorrect marketing/promotion, incorrect recommendations for product use, as well as reported incidents of questionable product quality and/or deliberate adulterations have also become frequent in recent years.

Direct and indirect high-performance liquid chromatographic enantioseparation of beta-amino acids.

Direct and indirect reversed-phase (RP) high-performance liquid chromatographic methods were developed for the separation of enantiomers of 18 unnatural beta-amino acids, including several beta-3-homo amino acids. The direct separations of the underivatized analytes were performed on chiral stationary phases (CSPs) containing macrocyclic glycopeptide antibiotic teicoplanin (Chirobiotic T column) and teicoplanin aglycone (Chirobiotic TAG column). The indirect method involved pre-column derivatization with a new chiral derivatizing agent (CDA), (S)-N-(4-nitrophenoxycarbonyl)phenylalanine methoxyethyl ester ((S)-NIFE), and subsequent separation of diastereomers on Discovery C18 and Hyperpep 300 C18 columns.

Application of a new chiral derivatizing agent to the enantioseparation of secondary amino acids.

A new chiral derivatizing agent, (S)-N-(4-nitrophenoxycarbonyl)phenylalanine methoxyethyl ester, (S)-NIFE, was applied for the high-performance liquid chromatographic separation of enantiomers of 19 unnatural secondary amino acids: proline, pipecolic acid analogues, piperazine-2-carboxylic acid, morpholine-3-carboxylic acid, thiomorpholine-3-carboxylic acid and analogues containing the 1,2,3,4-tetrahydroisoquinoline, 1,2,3,4-tetrahydronorharmane, 1,2,3,4-tetrahydro-2-carboline and 2-benzazepine skeletons. Excellent resolutions were achieved for most of the investigated compounds by using a reversed-phase mobile phase system. The conditions of separation were optimized by variation of the mobile phase composition.

Effects of temperature on retention of chiral compounds on a ristocetin A chiral stationary phase.

The isocratic retention of enantiomers of chiral analytes, i.e. tryptophan, 1,2,3,4-tetrahydroisoquinoline and gamma-butyrolac tone analogs, was studied on a ristocetin A chiral stationary phase at different temperatures and with different mobile phase compositions, using the reversed-phase, polar-organic and normal-phase modes.

Indirect high-performance liquid chromatographic separation of stereoisomers of beta-alkyl-substituted amino acids by the application of (S)-N-(4-nitrophenoxycarbonyl)phenylalanine methoxyethyl ester as chiral derivatizing agent.

The indirect high-performance liquid chromatographic enantioresolution of beta-alkyl-substituted analogues of tyrosine, phenylalanine, 1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid and tryptophan is reported. (S)-N-(4-Nitrophenoxycarbonyl)phenylalanine methoxyethyl ester, a recently developed chiral derivatizing agent, was used for pre-column derivatization of the investigated analytes. The diastereoisomers formed were analysed under reversed-phase conditions.