Kumar Sandeep, Anderson Kyle W
Institute for Bioscience and Biotechnology Research, National Institute of Standards and Technology and the University of Maryland, College Park, Rockville, Maryland 20850, United States.
National Institute of Standards and Technology, Bioprocess Measurements Group, Biomolecular Measurement Division, Gaithersburg, Maryland 20899, United States.
J Am Soc Mass Spectrom. 2025 Feb 5;36(2):340-345. doi: 10.1021/jasms.4c00411. Epub 2024 Dec 22.
Sample carryover is a common problem in hydrogen-deuterium exchange mass spectrometry, particularly because immobilized protease columns cannot withstand the high organic solvent concentrations typically used in liquid chromatography-mass spectrometry (LC-MS) for cleaning. Conventional cleaning methods using injections of guanidine HCl still suffer from carryover and may require four blanks after each sample run to fully remove carryover. We have implemented an additional LC pump to deliver customized wash solutions to protease and enzyme columns, and the associated LC capillaries to eliminate carryover. Pump-based washing using the protease-safe wash solutions tested herein was able to fully remove carryover with only one blank run. FOS-choline-12 was found to be the most effective component in wash solutions and even performed well alone at 0.1% volume concentration. Since the protease column washing is performed concurrently during the analytical gradient within a sample run, subsequent blank runs could be reduced from four to one and total run time could be reduced by up to 60%. Savings in total run time could more than double the productivity of data acquisition, which is imperative for pandemic preparedness and for acceleration of biotherapeutics development.
样品残留是氢-氘交换质谱分析中的一个常见问题,尤其是因为固定化蛋白酶柱无法承受液相色谱-质谱联用(LC-MS)清洗时通常使用的高有机溶剂浓度。使用盐酸胍进样的传统清洗方法仍然存在残留问题,每次样品分析后可能需要四个空白样来完全消除残留。我们增加了一个液相色谱泵,用于向蛋白酶柱和酶柱输送定制的清洗溶液,以及相关的液相色谱毛细管,以消除残留。使用本文测试的蛋白酶安全清洗溶液进行基于泵的清洗,只需一次空白运行就能完全消除残留。发现FOS-胆碱-12是清洗溶液中最有效的成分,即使在体积浓度为0.1%时单独使用也表现良好。由于蛋白酶柱清洗是在样品分析梯度过程中同时进行的,后续空白运行次数可以从四次减少到一次,总运行时间最多可减少60%。总运行时间的节省可以使数据采集的效率提高一倍以上,这对于大流行防范和生物治疗药物开发的加速至关重要。