Department of Clinical Studies, School of Veterinary Medicine, University of Pennsylvania, New Bolton Center Campus, Kennett Square, PA 19348, USA.
J Anal Toxicol. 2013 Mar;37(2):122-32. doi: 10.1093/jat/bks098. Epub 2013 Jan 11.
A method involving ultra high-performance liquid chromatography-tandem mass spectrometry was developed and validated for the analysis of capsaicin and dihydrocapsaicin in equine plasma. The analytes were recovered from plasma by liquid-liquid extraction using methyl tert-butyl ether and separated on a sub-2 micron column. The mobile phase was composed of 2 mM ammonium formate and methanol. A triple quadrupole mass spectrometer was used to detect the analytes in positive electrospray ionization mode with selected reaction monitoring. The limits of detection, quantification and confirmation for both analytes were 0.5, 1.0 and 2.5 pg/mL, respectively. The linear dynamic range of quantification was 1.0-1,000 pg/mL. During storage, both analytes in equine plasma were unstable at room temperature but stable at -20 and -70°C. The retention time and product ion ratios were employed as the criteria for confirmation of the presence of the analytes in plasma. The total analysis time was 2 min. The method is fast, selectively sensitive, reproducible, reliable and fully validated.
建立并验证了一种超高效液相色谱-串联质谱法，用于分析马血浆中的辣椒素和二氢辣椒素。用甲基叔丁基醚进行液液萃取从血浆中提取分析物，并在亚 2 微米柱上进行分离。流动相由 2 mM 甲酸铵和甲醇组成。采用正电喷雾电离模式，三重四极杆质谱仪以选择反应监测法检测分析物。两种分析物的检测限、定量下限和确证限分别为 0.5、1.0 和 2.5 pg/mL。定量的线性动态范围为 1.0-1,000 pg/mL。在室温下，马血浆中的两种分析物在储存过程中不稳定，但在-20°C 和-70°C 下稳定。保留时间和产物离子比被用作确认血浆中分析物存在的标准。总分析时间为 2 分钟。该方法快速、选择性灵敏、重现性好、可靠，且完全经过验证。
