School of Chemistry, Faculty of Engineering and Physical Sciences, University of Southampton, Highfield, Southampton, SO17 1BJ, UK.
Rapid Commun Mass Spectrom. 2020 Aug 30;34(16):e8848. doi: 10.1002/rcm.8848.
Fast and easily transferable chromatography/mass spectrometry assays were required to detect and quantify the amount of Bitrex™ and sodium saccharin in homemade facemask fit testing solutions.
Bitrex™ solutions were analysed using reversed-phase ultrahigh-performance liquid chromatography coupled with positive ion electrospray ionisation mass spectrometry (UHPLC/ESI-MS). Separation was achieved using a mobile phase gradient with an Acquity BEH C18-packed column. Sodium saccharin solutions were analysed using ultrahigh-performance supercritical fluid chromatography coupled with negative ion electrospray ionisation (UHPSFC/ESI-MS). Separation was achieved using isocratic elution with an Acquity UPC Torus Diol packed column and a methanol (25 mM ammonium acetate) co-solvent.
The calibration curves obtained using the ratio of the active compound to an internal standard generated linear regression values (R ) >0.99. Samples analysed prior to and after an autoclave sterilisation process and bottling gave repeatable measurements within 10% of the expected concentration.
The two assays afford a fast robust and quantitative analytical method for the detection of the active components used to test the efficacy of the homemade facemask testing solutions.
未加标签：需要快速且易于转换的色谱/质谱分析方法来检测和定量自制口罩贴合测试溶液中的 Bitrex™ 和糖精钠含量。
方法：采用反相超高效液相色谱-正离子电喷雾离子化质谱联用（UHPLC/ESI-MS）分析 Bitrex™溶液。采用 Accuuty BEH C18 填充柱的流动相梯度实现分离。采用超高效超临界流体色谱-负离子电喷雾离子化（UHPSFC/ESI-MS）分析糖精钠溶液。采用 Acquity UPC Torus Diol 填充柱和甲醇（25 mM 乙酸铵）共溶剂进行等度洗脱实现分离。
结果：使用活性化合物与内标物的比值得到的校准曲线产生了线性回归值（R）>0.99。在经过高压灭菌消毒和装瓶处理前后进行分析的样品，其测量结果在预期浓度的 10%以内具有可重复性。
结论：这两种分析方法提供了一种快速、稳健和定量的分析方法，可用于检测用于测试自制口罩测试溶液功效的活性成分。
