Analytical Sciences

Abstract − Analytical Sciences, 37(8), 1095 (2021).

Preparation of a New β-Cyclodextrin-bonded Chiral Stationary Phase with Thiocarbamated Benzamide Spacer for HPLC
Tianci ZHANG, Yazhou SHUANG, Hui ZHONG, Liang LI, and Laisheng LI
College of Chemistry, Nanchang University, No. 999, Xuefu Ave., Honggutan Dist., Nanchang 330031, China
A new β-cyclodextrin-bonded chiral stationary phase (TCDP) with a thiocarbamated benzamide spacer was prepared and evaluated on HPLC by separating a series of chiral pesticides and drugs. TCDP resolved all 24 analytes (11 triazoles, 8 flavanones and 5 β-blockers), and 18 of them were completely separated. The enantioresolution ranges were 1.45 – 3.33 for triazoles, 0.35 – 2.45 for flavanones and 1.26 – 1.58 for β-blockers. Among them the best resolution of tebuconazole was up to 3.33 within 13 min. Bitertanol (two chiral centers) and triticonazole with cis/trans isomers were separated into four peaks, respectively. TCDP could also completely resolve myclobutanil (Rs = 1.68), which was difficult to be separated on other CD-CSPs. Common CDSP only resolved a few analytes. The results showed that the thiocarbamated benzamide spacer of TCDP may provide a synergistic effect of hydrogen bonding and coordination. The spacer deserved full utilization, by which may avoid troublesome derivatization at low cost.