This paper aims to expand the range of matrix assisted laser desorption mass spectrometry analysis (MALDI MS) as a tool to establish the reaction kinetics for a particular case study: the synthesis of β-cyclodextrin-oligolactide (CDLA) derivatives through solution ring opening oligomerization (ROO) of d,l-lactide (LA) initiated by β-cyclodextrin (β-CD). Specifically, MALDI MS was used to estimate the molecular weight averages minute changes during the synthesis for a better understanding of the chemical process. The MALDI MS data was compared with ¹H NMR for determining the DL-Lactide conversion rate and an excellent agreement level was established. The synthesis process was further studied by observing the effects of the reaction parameters with a special focus on the solvent influence. Thus, we observed that the ROO performed in dimethylformamide and N-methyl-2-pyrrolidone proceeds faster in comparison with dimethylsulfoxide due to an activation process in the LA ring opening reaction. The activation is produced by the amines resulted from the cleavage of the amide bonds in the presence of the β-CD or CDLA derivatives. The products of the degradation process were identified in the MS spectra and structurally confirmed through MS fragmentation experiments.

本文旨在扩大基质辅助激光解吸质谱分析 (MALDI MS) 的范围，作为建立特定案例研究的反应动力学的工具：通过溶液开环低聚反应合成 β-环糊精-低聚乳酸 (CDLA) 衍生物(ROO)由 β-环糊精 (β-CD) 引发的d , l-丙交酯 (LA)。具体来说，MALDI MS 用于估计合成过程中平均分子量的微小变化，以便更好地了解化学过程。MALDI MS 数据与¹确定 DL-丙交酯转化率的 H NMR 建立了良好的一致性水平。通过观察反应参数的影响，特别关注溶剂的影响，进一步研究了合成过程。因此，我们观察到由于 LA 开环反应中的活化过程，在二甲基甲酰胺和 N-甲基-2-吡咯烷酮中进行的 ROO 与二甲基亚砜相比进行得更快。在 β-CD 或 CDLA 衍生物存在的情况下，酰胺键断裂产生的胺产生活化作用。降解过程的产物在 MS 光谱中得到鉴定，并通过 MS 碎裂实验在结构上得到证实。