Stir membrane liquid phase microextraction of tetracyclines using switchable hydrophilicity solvents followed by high-performance liquid chromatography.

A novel approach for stir membrane liquid phase microextraction of tetracyclines from biological fluids was developed. The microextraction procedure assumed in situ formation of microdroplets of a hydrophobic medium-chain fatty acid (extraction solvent) from homogeneous sample solution containing water-soluble medium-chain fatty acid salt by acidification and simultaneous analytes extraction and organic phase separation into pores of stir membrane disk. Obtained large surface area between the extraction solvent and aqueous phase and high porosity of the membrane provided fast extraction and phase separation (extraction time - 5 min) and reducing extraction solvent volume to the order of several µL. The developed approach was applied for the HPLC-UV determination of tetracycline, oxytetracycline and chlortetracycline in biological fluids samples. The calibration graphs were linear over the concentration ranges of 0.1-100 mg L-1 for oxytetracycline, tetracycline and chlortetracycline. Regression coefficients were in the range from 0.994 to 0.998. The LOD values, calculated from the blank tests based on 3σ, were 30 µg L-1 for tetracycline, oxytetracycline and chlortetracycline. The RSD values expressing intra-day and inter-day repeatability were lower than 5% and 8%, respectively.

Crystal structure of a 2:1 co-crystal of meloxicam with acetyl-endi-carb-oxy-lic acid.

The pharmaceutical 2:1 co-crystal of meloxicam [MXM; systematic name: 4-hy-droxy-2-methyl-N-(5-methyl-thia-zol-2-yl)-2H-1,2-benzo-thia-zine-3-carboxamide 1,1-dioxide] with acetyl-enedi-carb-oxy-lic acid (ACA; systematic name: but-2-ynedioic acid), crystallizes with one MXM mol-ecule and half an ACA mol-ecule in the asymmetric unit, C14H13N3O4S2·0.5C4H2O4. The mid-point of the triple bond of ACA is located on an inversion centre. In the crystal, the two stereoisomers of MXM with respect to the N atom of the sulfonamide group are related by the inversion centre. The carbonyl and hy-droxy groups belonging to the MXM mol-ecule are involved in an intra-molecular O-H⋯O hydrogen bond. The structure-forming motif includes two MXM mol-ecules linked via an ACA conformer through N-H⋯O and O-H⋯N hydrogen bonds, similar to MXM co-crystals with other di-carb-oxy-lic acids.