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手性分离使用环糊精作为流动相添加剂在开管液相色谱中与伪相涂层。

Chiral separation using cyclodextrins as mobile phase additives in open-tubular liquid chromatography with a pseudophase coating.

机构信息

Australian Centre for Research on Separation Science, School of Natural Sciences-Chemistry, University of Tasmania, Hobart, Tasmania, Australia.

出版信息

J Sep Sci. 2022 Mar;45(6):1195-1201. doi: 10.1002/jssc.202100835. Epub 2022 Jan 22.

DOI:10.1002/jssc.202100835
PMID:35014193
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9304321/
Abstract

The chiral separation of various analytes (dichlorprop, mecoprop, ibuprofen, and ketoprofen) was demonstrated with different cyclodextrins as mobile phase additives in open-tubular liquid chromatography using a stationary pseudophase semipermanent coating. The stable coating was prepared by a successive multiple ionic layer approach using poly(diallyldimethylammonium chloride), polystyrene sulfonate, and didodecyldimethyl ammonium bromide. Increasing concentrations (0-0.2 mM) of various native and derivatized cyclodextrins in 25 mM sodium tetraborate (pH 9.2) were investigated. Chiral separation was achieved for the four test analytes using 0.05-0.1 mM β-cyclodextrin (resolution between 1.11 and 1.34), γ-cyclodextrin (resolution between 0.78 and 1.27), carboxymethyl-β-cyclodextrin (resolution between 1.64 and 2.59), and 2-hydroxypropyl-β-cyclodextrin (resolution between 0.71 and 1.76) with the highest resolutions obtained with 0.1 mM carboxymethyl-β-cyclodextrin. %RSD values were <10%. This is the first demonstration of chiral open-tubular liquid chromatography using achiral chromatographic coatings and cyclodextrins as mobile phase additives.

摘要

采用固定的伪永久相涂层,在开管液相色谱中,用不同的环糊精作为流动相添加剂,展示了各种分析物(二氯丙酸、麦草畏、布洛芬和酮洛芬)的手性分离。通过使用聚(二烯丙基二甲基氯化铵)、聚苯乙烯磺酸盐和双十二烷基二甲基溴化铵的连续多次离子层方法制备了稳定的涂层。考察了在 25 mM 四硼酸钠(pH 9.2)中不同浓度(0-0.2 mM)的各种天然和衍生化环糊精。使用 0.05-0.1 mM β-环糊精(分辨率在 1.11 和 1.34 之间)、γ-环糊精(分辨率在 0.78 和 1.27 之间)、羧甲基-β-环糊精(分辨率在 1.64 和 2.59 之间)和 2-羟丙基-β-环糊精(分辨率在 0.71 和 1.76 之间)实现了对四种测试分析物的手性分离,最高分辨率为 0.1 mM 羧甲基-β-环糊精。%RSD 值<10%。这是首次使用非手性色谱涂层和环糊精作为流动相添加剂进行手性开管液相色谱的演示。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9590/9304321/af872e3c9caa/JSSC-45-1195-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9590/9304321/19a5cbc23a80/JSSC-45-1195-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9590/9304321/0c5b70045374/JSSC-45-1195-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9590/9304321/af872e3c9caa/JSSC-45-1195-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9590/9304321/19a5cbc23a80/JSSC-45-1195-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9590/9304321/0c5b70045374/JSSC-45-1195-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9590/9304321/af872e3c9caa/JSSC-45-1195-g003.jpg

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