Nyadong Leonard, Hohenstein Edward G, Johnson Kristin, Sherrill C David, Green Michael D, Fernández Facundo M
School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, GA 30332, USA.
Analyst. 2008 Nov;133(11):1513-22. doi: 10.1039/b809471c. Epub 2008 Aug 1.
Competitive host-guest chemistry on a desorption electrospray ionization mass spectrometry (DESI MS) platform is presented here as the basis for a rapid and quantitative screening method for assessing the quality of Tamiflu capsules with minimal sample preparation. Oseltamivir, the active ingredient in Tamiflu, is an orally active neuraminidase inhibitor antiviral. The high cost and demand for this drug has made it a target for counterfeiters, and reports of counterfeit Tamiflu capsules have already appeared. This urges the development of rapid and sensitive tools for Tamiflu authentication. The method presented here is based on the selective recognition of oseltamivir by crown ethers added to the DESI spray solvent. Crown ethers with various ring sizes were evaluated, all being observed to form stable host-guest complexes with protonated oseltamivir. The relative gas phase stability of each of the host-guest complexes was assessed and the results compared with dispersion-corrected density functional theory. Competive experiments with various pairs of crown ethers were used to assess the relative binding selectivities for oseltamivir. The abundance ratio of the formed complexes was observed to be dependent on the amount of analyte present on the surface of the sample, and independent of DESI geometric factors. These competitive reactions were then successfully tested as a means for the rapid quantitation of oseltamivir by reactive DESI MS without the need for an internal standard.
本文介绍了一种基于解吸电喷雾电离质谱(DESI MS)平台的竞争性主客体化学方法,作为一种快速定量筛选方法的基础,用于在最小化样品制备的情况下评估达菲胶囊的质量。达菲中的活性成分奥司他韦是一种口服活性神经氨酸酶抑制剂抗病毒药物。这种药物的高成本和高需求使其成为造假者的目标,假冒达菲胶囊的报道已经出现。这促使开发快速灵敏的达菲鉴别工具。本文提出的方法基于向DESI喷雾溶剂中添加冠醚对奥司他韦的选择性识别。评估了各种环大小的冠醚,发现它们都能与质子化的奥司他韦形成稳定的主客体复合物。评估了每个主客体复合物的相对气相稳定性,并将结果与色散校正密度泛函理论进行了比较。使用各种冠醚对进行竞争实验,以评估对奥司他韦的相对结合选择性。观察到形成的复合物的丰度比取决于样品表面存在的分析物量,并且与DESI几何因素无关。然后,这些竞争反应作为一种通过反应性DESI MS快速定量奥司他韦的方法成功进行了测试,无需内标。