Department of Analytical Chemistry, Faculty of Science, P.J. Šafárik University, Moyzesova 11, SK-040 01, Košice, Slovak Republic.
Department of Analytical Chemistry, Faculty of Science, P.J. Šafárik University, Moyzesova 11, SK-040 01, Košice, Slovak Republic.
J Pharm Biomed Anal. 2020 Oct 25;190:113549. doi: 10.1016/j.jpba.2020.113549. Epub 2020 Aug 15.
New, sensitive and rapid chiral HPLC method for enantioseparation and determination of widely used hypnotic drug, zopiclone, was developed. Enantioseparation was achieved on the immobilized amylose based Lux i-Amylose 1 column in polar organic mode in less than 7 min. The effects of the mobile phase composition, type and content of major components as well as acid/base ratio and column temperature on the retention and enantioseparation were investigated. The mobile phase consisted of acetonitril and methanol with small addition of triethylamine and acetic acid with a flow rate of 1 mL min. Calibration curves of both zopiclone enantiomers were linear over the concentration range of 5-125 μg mL. The limits of detection and quantification for (R)-zopiclone were 5 and 15 ng mL and for (S)-zopiclone were 7 and 21 ng mL, respectively. It was demonstrated that the proposed method was selective, precise and robust. Finally, the validated method was applied to the determination of zopiclone enantiomers in the commercial tablets.
开发了一种新的、灵敏的、快速的手性 HPLC 方法，用于广泛使用的催眠药物佐匹克隆对映体的分离和测定。在极性有机模式下，在手性固定相 Lux i-Amylose 1 柱上不到 7 分钟即可实现对映体分离。考察了流动相组成、主要成分的类型和含量、酸碱比和柱温对保留和对映体分离的影响。流动相由乙腈和甲醇组成，加入少量三乙胺和乙酸，流速为 1 mL min。两种佐匹克隆对映体的校准曲线在 5-125 μg mL 的浓度范围内呈线性。（R）-佐匹克隆的检测限和定量限分别为 5 和 15 ng mL，（S）-佐匹克隆分别为 7 和 21 ng mL。结果表明，该方法具有选择性、精确性和稳健性。最后，验证后的方法用于测定市售片剂中佐匹克隆对映体的含量。
