新型芳香酶抑制剂在反相模式下基于纤维素和直链淀粉的手性固定相上的高效液相色谱对映体拆分

HPLC enantiomeric resolution of novel aromatase inhibitors on cellulose- and amylose-based chiral stationary phases under reversed phase mode.

作者信息

Aboul-Enein H Y, Ali I, Gübitz G, Simons C, Nicholls P J

机构信息

Pharmaceutical Analysis Laboratory, Biological and Medical Research Department (MBC-03), King Faisal Specialist Hospital and Research Center, Riyadh, Saudi Arabia.

出版信息

Chirality. 2000 Nov;12(10):727-33. doi: 10.1002/1520-636X(2000)12:10<727::AID-CHIR5>3.0.CO;2-T.

DOI:10.1002/1520-636X(2000)12:10<727::AID-CHIR5>3.0.CO;2-T

PMID:11054831

Abstract

The chiral resolution of seven aromatase inhibitors (four triazole derivatives (Ia, Ib, Ic, and Id) and three tetrazole derivatives (IIa, IIb, and IIc)) was achieved on Chiralcel OJ-R [cellulose tris (4-methyl benzoate)], Chiralcel OD-RH [cellulose tris (3,5-dimethylphenyl carbamate)], and Chiralpak AD-RH [amylose tris (3,5-dimethylphenyl carbamate)] chiral stationary phases. The mobile phases used were A: 2-PrOH-MeCN (90:10, v/v); B: 2-PrOH-MeCN (50:50, v/v); C: MeCN-H(2)O (50:50, v/v); D: MeCN-H(2)O (80:20, v/v); and E: MeCN-H(2)O (95:05, v/v). The flow rate was 0.5 mL/min for all the mobile phases. The resolution capability of these chiral stationary phases were in the order Chiralpak AD-RH > Chiralcel OD-RH > Chiralcel OJ-R. The values of alpha and Rs of the resolved enantiomers of the aromatase inhibitors varied from 1.02-5.63 and 1. 12-6.72, respectively.

摘要

在Chiralcel OJ-R [三（4-甲基苯甲酸）纤维素]、Chiralcel OD-RH [三（3,5-二甲基苯基氨基甲酸酯）纤维素]和Chiralpak AD-RH [三（3,5-二甲基苯基氨基甲酸酯）直链淀粉]手性固定相上实现了7种芳香酶抑制剂（4种三唑衍生物（Ia、Ib、Ic和Id）和3种四唑衍生物（IIa、IIb和IIc））的手性拆分。所使用的流动相为：A：2-丙醇-乙腈（90:10，v/v）；B：2-丙醇-乙腈（50:50，v/v）；C：乙腈-水（50:50，v/v）；D：乙腈-水（80:20，v/v）；E：乙腈-水（95:05，v/v）。所有流动相的流速均为0.5 mL/min。这些手性固定相的拆分能力顺序为Chiralpak AD-RH > Chiralcel OD-RH > Chiralcel OJ-R。芳香酶抑制剂对映体拆分后的α值和Rs值分别在1.02 - 5.63和1.12 - 6.72之间。