Acetylcholinesterase (AChE) and α-glucosidase (α-glu) are key target enzymes in the search for novel strategies in the treatment of Alzheimer’s disease and type II diabetes. Therefore, methods to assess the enzyme inhibition are of great value in the research field. Here is proposed a novel a dual electrophoretically-mediated microanalysis for the simultaneous determination of both enzymes’ activity. In order to do so, the various solutions required for both assays were introduced in the capillary electrophoresis system using the multiple injections approach. Enzymatic kinetic parameters were tested, K_m for AChE and α-glu were 3.81 and 0.43 mmol L^-1. K_i values were 4.27 μmol L^-1 for neostigmine (an AChE inhibitor) and 0.40 mmol L^-1 for acarbose (an α-glu inhibitor). Results of IC₅₀ (concentration for 50 % of inhibition) were 5.11 ± 0.47 μmol L^-1 and 0.58 ± 0,02 mmol L^-1 for neostigmine and acarbose, respectively. All parameters (except for K_i of neostigmine) were comparable with the literature, indicating a good reliability of the proposed method to evaluate these enzymes activity. Total time analysis was approximately 10 min, being possible to perform around 12 enzymatic assays per hour, with low sample and reagent consumption, thus satisfying some of the principles of green chemistry. The method was applied to evaluate 10 phenolic compounds, of wich p-coumaric acid showed the best inhibitory activity for AChE (40.14 ± 4.75 % at 10 mg L^-1); and quercetin for α-glu (46.53 ± 4.90 % at 10 mg L^-1).

乙酰胆碱酯酶（AChE）和α-葡萄糖苷酶（α-glu）是寻找治疗阿尔茨海默氏病和II型糖尿病的新策略时的关键靶酶。因此，评估酶抑制作用的方法在研究领域具有重要价值。在此提出了一种新颖的双重电泳介导的微量分析方法，用于同时测定两种酶的活性。为此，使用多次进样方法将两种测定所需的各种溶液引入毛细管电泳系统。测试了酶动力学参数，AChE和α-glu的K _m为3.81和0.43 mmol L ^-1。K _i值为4.27μmolL ^-1对于新斯的明（一种AChE抑制剂）为0.40 mmol L ^-1（对于阿卡波糖（一种α-glu抑制剂））。新斯的明和阿卡波糖的IC ₅₀结果（抑制50％的浓度）分别为5.11±0.47μmolL ^-1和0.58±0,02 mmol L ^-1。所有参数（除了ķ_我新斯的明）为与文献相媲美，表明所提出的方法来评价这些酶的活性的一个良好的可靠性。总时间分析约为10分钟，每小时可以进行约12次酶促测定，而样品和试剂的消耗量却很低，因此满足了绿色化学的某些原理。施加到评估10的酚类化合物的方法，至极的p-香豆酸对AChE表现出最佳的抑制活性（10 mg L ^-1时为40.14±4.75％）；和槲皮素用于α-glu（在10 mg L ^-1时为46.53±4.90％）。