GC法测定(1R,2R)-(-)-1,2-环己二胺中S,S对映异构体  

Determination of S,S-enantiomer in(1R,2R)-(-)-1,2-cyclohexanediamine by GC

作　　者：朱圣亮[1] 宋晓光[1] 韩斌[1] 祝传斌 李语如[1] 

机构地区：[1]江苏恒瑞医药股份有限公司研究所,江苏连云港222002

出　　处：《药学进展》2009年第4期174-177,共4页Progress in Pharmaceutical Sciences

摘　　要：目的:建立GC法,测定(1R,2R)-(-)-1,2-环己二胺中S,S对映异构体。方法:用三氟乙酸酐对1,2-环己二胺进行柱前衍生化。色谱柱:CHIRALDEXTMB-DP二丙酰化β-环糊精手性毛细管柱(30 m×0.25 mm),检测器:FID,进样口及检测器温度:200℃,柱温:175℃,载气:氮气,流速:3.0 mL.min-1,分流比:50∶1,进样量:1.0μL。结果:1,2-环己二胺的R,R与S,S对映异构体衍生物达到基线分离;S,S对映异构体定量限和检测限分别为2.2和0.66 mg.L-1,平均回收率为96.2%,RSD为2.1%(n=6)。结论:本法能较为准确、快速、有效地分离测定(1R,2R)-(-)-1,2-环己二胺中S,S对映异构体。Objective： To establish a GC method for determination of S, S-enantiomer in （ 1R, 2R） -（ - ） -1, 2-cyclohexanediamine. Methods： The pre-column derivatization of 1, 2-cyclohexanediamine was conducted with TFAA. The GC condition was used as follows： CHIRALDEX^TM B-DP capillary column （ β-cyclodextrin, dipropionyl, 30 m × 0.25 mm）, a FID detector, a sampling/detector temperature of 200 ℃, a column temperature of 175 ℃, N2 as carrier gas, a flow rate of 3.0 mL·min^-1, a split ratio of 50 ： 1 and a sampling volume of 1.0μL. Results： The baseline resolution was achieved between the derivatives of S, S-and R, R-enantiomers of 1, 2-cyclohexanediamine. The quantitative and detective limits were 2.2 and 0. 66 mg·L-1 respectively and the average recovery was 96.2% with RSD of 2.1% （n =6） for the S, S-enantiomer. Conclusion： The method is acurate, rapid and effective for the determination of S, S-enantiomer in （ 1R, 2R） -（ - ） -1,2-cyclohexanediamine.

关 键 词：气相色谱 (1R 2R)-(-)-1 2-环己二胺 S S对映异构体 柱前衍生化 含量测定 

分 类 号：TQ236[化学工程—有机化工]