Melanson J E, Wong B L, Boulet C A, Lucy C A
Department of Chemistry, University of Alberta, Edmonton, Canada.
J Chromatogr A. 2001 Jun 22;920(1-2):359-65. doi: 10.1016/s0021-9673(01)00685-9.
Capillary electrophoresis coupled with indirect UV absorbance detection was employed for the determination of the chemical warfare agent degradation products: methylphosphonic acid, ethyl methylphosphonate, isopropyl methylphosphonate, and pinacolyl methylphosphonate. Glutamic acid was used as a buffering agent at its isoelectric point (pH 3.22). In its zwitterionic form, glutamic acid does not act as a competing co-anion in the system, thus providing buffering capacity while maintaining high sensitivity. The indirect probe (phenylphosphonic acid) concentration was lowered to 1 mM from the 10 mM in previous literature studies, further enhancing sensitivity. Detection limits of 2 microM were achieved with hydrodynamic injection and up to 100-fold lower using electrokinetic injection. The increased buffering capacity of this system over previous methods led to migration time reproducibility RSD values of 0.18 to 0.22%. This represents a 10-fold improvement in reproducibility over previous studies with comparable or improved sensitivity.
甲基膦酸、甲基膦酸乙酯、甲基膦酸异丙酯和甲基膦酸频哪酯。谷氨酸在其等电点(pH 3.22)用作缓冲剂。以两性离子形式存在时,谷氨酸在体系中不充当竞争性共阴离子,因此在保持高灵敏度的同时提供缓冲能力。间接探针(苯膦酸)浓度从先前文献研究中的10 mM降至1 mM,进一步提高了灵敏度。采用流体动力进样时检测限为2 μM,采用电动进样时检测限可低至100倍。该系统相对于先前方法增强的缓冲能力使迁移时间重现性的相对标准偏差(RSD)值为0.18%至0.22%。这表明与先前研究相比,重现性提高了10倍,且灵敏度相当或有所提高。