Sample Pretreatment and Determination of Non Steroidal Anti-Inflammatory Drugs (NSAIDs) in Pharmaceutical Formulations and Biological Samples (Blood, Plasma, Erythrocytes) by HPLC-UV-MS and μ-HPLC

Mohamed      Sultan; Gunther      Stecher; Wolfgang   M.   Stoggl; Rania      Bakry; P.      Zaborski; C.   W.   Huck; Nagla   M.   El Kousy; Gunther   K.   Bonn

Abstract

The article discusses the qualitative and quantitative determination of non-steroidal antiinflammatory drugs like salicin, salicylic acid, tenoxicam, ketorolac, piroxicam, tolmetin, naproxen, flurbiprofen, diclofenac and ibuprofen by reversed phase high performance liquid chromatography (RP-HPLC) and micro-HPLC (μ-HPLC) hyphenated with UV-absorbance and mass spectrometric detection. Both detection methods delivered calibration plots with good linearity (r2 < 0.9800), limits of detection in the low nanogram range and recovery rates between 94 and 104 %. For the analysis of biological samples such as blood, plasma and erythrocytes liquid-liquid extraction (LLE) and solid phase extraction (SPE) on the basis of new synthesized glycidylmethacrylate / divinylbenzene copolymer (GMA / DVB) particles and commercially available material on the basis of poly(divinylbenzene-co-N-vinylpyrrolidone) copolymer were investigated. Finally the use of a μ-HPLC system with separation columns in the range of 8 cm × 200 µm I.D. for the determination of non-steroidal anti-inflammatory drugs (NSAIDs) is presented, emphasizing on the type of column and sample amount needed.

Keywords: antirheumatic, hplc, mass spectrometry, blood, plasma, erythrocytes, extraction, glycidylmetharylate/divinylbenzene copolymer