Department of Chemistry "Sapienza" University of Rome, P.le Aldo Moro 5, 00185 Rome, Italy.
Istituto per i Sistemi Biologici (ISB), CNR- Consiglio Nazionale delle Ricerche, Via Salaria Km 29,300, 00015 Monterotondo (Rome), Italy.
J Chromatogr A. 2022 Jun 21;1673:463128. doi: 10.1016/j.chroma.2022.463128. Epub 2022 May 8.
In this paper enantiomers of selected chiral agrochemicals representing various structural classes were separated by using nano-liquid chromatography (nano-LC) and capillary electrochromatography (CEC) employing a capillary column packed with silica particles containing immobilized amylose tris(3‑chloro-5-methylphenylcarbamate) (i-ADMPC) as a chiral selector (CS). Special attention was paid to peak dispersion in nano-LC and CEC instruments used in order to make comparison between these two techniques more reliable. Enantioseparations were studied utilizing methanol (MeOH) or acetonitrile-water (ACNHO), both containing 5 mM of ammonium acetate as the mobile phases (MPs). The tested chiral stationary phase (CSP), containing 20% (w/w) of the neutral CS onto native silica, allowed the generation of sufficiently strong electroosmotic flow (EOF) to observe separation of enantiomers of studied agrochemicals in a reasonable time also in CEC mode. Modestly higher efficiencies and enantioresolutions were obtained in CEC than in nano-LC. Just a moderate preference of CEC over nano-LC in this particular study can be explained with a significant mass transfer resistance through the CSP that is caused due to high content of the CS in CSP.
本文使用纳米液相色谱（nano-LC）和毛细管电色谱（CEC），通过在填充有固定化直链淀粉三（3-氯-5-甲基苯基氨基甲酸酯）（i-ADMPC）作为手性选择剂（CS）的毛细管柱上分离各种结构类型的手性农用化学品对映异构体。特别关注了在用于比较这两种技术的 nano-LC 和 CEC 仪器中峰展宽的问题。使用甲醇（MeOH）或乙腈-水（ACNHO）作为流动相（MPs），其中均含有 5 mM 乙酸铵，研究了对映异构体的分离。测试的手性固定相（CSP），在天然硅胶上含有 20%（w/w）的中性 CS，允许产生足够强的电动流（EOF），以便在 CEC 模式下也能在合理的时间内观察到研究农用化学品的对映异构体的分离。在 CEC 中获得的效率和对映选择性略高于 nano-LC。在这项特定的研究中，CEC 只是适度优于 nano-LC，可以解释为由于 CSP 中 CS 含量高而导致通过 CSP 的传质阻力很大。
