Preparative enantiomeric separation of potent AMP-activated protein kinase activator by HPLC on amylose-based chiral stationary phase. Determination of enantiomeric purity and assignment of absolute configuration.

The development of high performance liquid chromatography method on amylose-based stationary phases (Chiralpak AD) has permitted to achieve the preparative enantioseparation of one benzimidazole derivative, potent-AMP-kinase (AMPK) activator with satisfactory yields. Analytical enantioseparation method was optimized and validated to determine the enantiomeric purity. Using the UV detection, repeatability, limits of detection (LD) and quantification (LQ) were determined.

Bis(ammonium) tris(hexaaquamagnesium) tetrakis(hydrogen phosphite).

The structure of the title compound, (NH4)2[Mg(H2O)6]3(HPO3)4, consists of [Mg(H2O)6]2+ and (NH4)+ cations and (HPO3)2- anions held together by an intricate network of hydrogen bonds involving all H atoms except for one linked directly to a P atom. The Mg2+ cations are octahedrally coordinated by six water molecules. One of the Mg atoms is located on a site with 2/m symmetry, whereas the other Mg atom and the P and N atoms occupy sites with m symmetry.

Preparative enantiomeric separation of new aromatase inhibitors by HPLC on polysaccharide-based chiral stationary phases: Determination of enantiomeric purity and assignment of absolute stereochemistry by X-ray structure analysis.

The development of high-performance liquid chromatography methods on polysaccharide-based stationary phases (cellulose or amylose derivatives) has permitted preparative enantioseparations of various 6-[1(imidazol-1-yl)-1-phenylmethyl]-3-methyl-1,3-benzoxazol-2(3H)-one and 6-[1(imidazol-1-yl)-1-phenylmethyl]-3-methyl-1,3-benzothiazol-2(3H)-one, aromatase inhibitors, with satisfactory yields. Analytical enantioseparation methods using both UV and evaporative light-scattering detection (ELSD) were validated to determine the enantiomeric purity of these compounds. Using UV detection, linear calibration curves in the range from 4 x 10(-6) to 4.

Preparative HPLC separation of methoxytetralins, ligands for melatonin receptors, containing two chiral centers with polysaccharide chiral stationary phases. Determination of enantiomeric purity.

Preparative chromatography was used to obtain approximately 200 mg of each of the four individual isomers of the three methoxytetrahydronaphthalenic derivatives, new agonist and antagonist ligands for melatonin receptors to be tested for binding. The mobile and stationary phases were chosen to achieve best resolution in shorter runtime. Enantiomeric purity was verified and quantified using normal and reversed phase methodology on cellulose CSPs.