Department of Molecular Biosciences and Bioengineering, University of Hawaii at Manoa, HI 96822, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Oct 1;906:58-62. doi: 10.1016/j.jchromb.2012.08.020. Epub 2012 Aug 21.
An aqueous normal phase (ANP) liquid chromatography coupled with a hybrid quadrupole time-of-flight mass spectrometry (ANP-LC-micrOTOFQ) method was used for the determination of zanamivir in human serum. Zanamivir was extracted with methanol from protein-precipitated human serum samples and further purified with SCX solid-phase extraction cartridges. Scherzo SM-C18, Agilent Zorbax SB-Aq, Cogent Diamond Hydride, Cogent Bidentate and Luna HILIC columns were compared and optimized for the retention and separation of zanamivir and the Luna HILIC and Diamond Hydride columns exhibited the best retention of zanamivir. The former provided a shorter retention time, a sharper peak and relatively high sensitivity, whereas the latter exhibited a longer retention time and less matrix interference. The analytical range of the calibration curve was between 5 and 1000 ng/mL.
采用水相正相(ANP)液相色谱-混合四极杆飞行时间质谱(ANP-LC-micrOTOFQ)法测定人血清中的扎那米韦。扎那米韦从蛋白沉淀的人血清样品中用甲醇提取,并用 SCX 固相萃取小柱进一步纯化。对 Scherzo SM-C18、Agilent Zorbax SB-Aq、Cogent Diamond Hydride、Cogent Bidentate 和 Luna HILIC 柱进行了比较和优化,以实现扎那米韦的保留和分离,其中 Luna HILIC 和 Diamond Hydride 柱对扎那米韦的保留效果最好。前者提供了较短的保留时间、更尖锐的峰和相对较高的灵敏度,而后者则具有较长的保留时间和较少的基质干扰。校准曲线的分析范围为 5 至 1000ng/mL。