Harry Emma L, Reynolds James C, Bristow Anthony W T, Wilson Ian D, Creaser Colin S
Centre for Analytical Science, Department of Chemistry, Loughborough University, Loughborough LE11 3TU, UK.
Rapid Commun Mass Spectrom. 2009 Sep;23(17):2597-604. doi: 10.1002/rcm.4152.
The direct analysis of pharmaceutical formulations and active ingredients from non-bonded reversed-phase thin layer chromatography (RP-TLC) plates by desorption electrospray ionisation (DESI) combined with ion mobility mass spectrometry (IM-MS) is reported. The analysis of formulations containing analgesic (paracetamol), decongestant (ephedrine), opiate (codeine) and stimulant (caffeine) active pharmaceutical ingredients is described, with and without chromatographic development to separate the active ingredients from the excipient formulation. Selectivity was enhanced by combining ion mobility and mass spectrometry to characterise the desorbed gas-phase analyte ions on the basis of mass-to-charge ratio (m/z) and gas-phase ion mobility (drift time). The solvent composition of the DESI spray using a step gradient was varied to optimise the desorption of active pharmaceutical ingredients from the RP-TLC plates. The combined RP-TLC/DESI-IM-MS approach has potential as a rapid and selective technique for pharmaceutical analysis by orthogonal gas-phase electrophoretic and mass-to-charge separation.
报道了通过解吸电喷雾电离（DESI）结合离子淌度质谱（IM-MS）对非键合反相薄层色谱（RP-TLC）板上的药物制剂和活性成分进行直接分析。描述了对含有镇痛剂（对乙酰氨基酚）、减充血剂（麻黄碱）、阿片类药物（可待因）和兴奋剂（咖啡因）活性药物成分的制剂的分析，有或没有进行色谱展开以将活性成分与辅料制剂分离。通过结合离子淌度和质谱，基于质荷比（m/z）和气相离子淌度（漂移时间）对解吸的气相分析物离子进行表征，从而提高了选择性。使用阶梯梯度改变DESI喷雾的溶剂组成，以优化活性药物成分从RP-TLC板上的解吸。RP-TLC/DESI-IM-MS联用方法作为一种通过正交气相电泳和质荷分离进行药物分析的快速且选择性技术具有潜力。
