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A rapid, precise, specific, and accurate Electrospray Ionisation Tandem Mass Spectrometry (ESI-MS / MS) method has been developed and subsequently validated, for the determination of pregabalin (PB) in human plasma. Gabapentin (GB) was used as the internal standard. PB and GB were extracted from the plasma using a combination of deproteinization, using 0.1% formic acid and liquid–liquid extraction, using methylene chloride. PB and GB were separated using the Hypurity advance column (50 mm × 4.6 mm, 5 μm) and mobile phase, consisting of methanol : 0.1% formic acid (80:20 v / v). PB was determined by using ESI-MS / MS in positive ion mode, with the help of the API 2000 spectrophotometer, operated in a multiple reaction monitoring mode. The parent-to-product ion combination of m / z 160.2→55.1 and 172.2→95.0 was used to quantify PB and GB, respectively. The assay was validated in the concentration range of 99.79 – 4019.90 ng / mL for PB. The limit of quantification (LOQ) was identifiable and reproducible at 99.79 ng / mL. The method has been successfully applied to study the pharmacokinetics of PB in healthy male volunteers.

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Novel mononuclear oxovanadium(IV) and manganese(III) complexes [VO(L 1 ) 2 ·H 2 O] (1); [VO(L 2 ) 2 ·H 2 O] (2); [VO(L 3 ) 2 ·H 2 O] (3); [Mn(L 1 ) 2 ]ClO 4 ·H 2 O (4); [Mn(L 2 ) 2 ] ClO 4 ·H 2 O (5); [Mn(L 3 ) 2 ]ClO 4 ·H 2 O (6) were prepared by condensation of 1 mol of VOSO 4 ·5H 2 O or Mn(OAc) 3 · 2H 2 O with 2 mol of ligand HL 1 , HL 2 or HL 3 (where HL 1-5-methyl-2-p-tolyl-2,4-dihydro-pyrazol-3-one; HL 3 = 4-{4-[(2-hydroxy-ethyl-amino)-methyl]-3-methyl-5-oxo-4,5-dihydropyrazol-1-yl} benzene sulfonic acid). The resulting complexes were characterized by elemental analyses, molar conductance, magnetic and decomposition temperature measurements, electron spin resonance, FAB mass, IR and electronic spectral studies. From TGA, DTA and DSC, the thermal behaviour and degradation kinetic were studied. Electronic spectra and magnetic susceptibility measurements indicate distorted octahedral stereochemistry of oxovanadium(IV) complexes and regular octahedral stereochemistry of manganese(III) complexes. Hamiltonian and bonding parameters found from ESR spectra indicate the metal ligand bonding is partial covalent. The X-ray single