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GC法测定(1R,2R)-(-)-1,2-环己二胺中S,S对映异构体
引用本文:朱圣亮,宋晓光,韩斌,祝传斌,李语如.GC法测定(1R,2R)-(-)-1,2-环己二胺中S,S对映异构体[J].药学进展,2009,33(4):174-177.
作者姓名:朱圣亮  宋晓光  韩斌  祝传斌  李语如
作者单位:江苏恒瑞医药股份有限公司研究所,江苏,连云港222002
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:CHIRALDEX^TM B-DP二丙酰化B-环糊精手性毛细管柱(30m×0.25mm),检测器:FID,进样口及检测器温度:200℃,柱温:175℃,载气:氮气,流速:3.0mL·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0.66mg·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。

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

Determination of S,S-enantiomer in (1R,2R)-(-)-1,2-cyclohexanediamine by GC
ZHU Sheng-liang,SONG Xiao-guang,HAN Bin,ZHU Chuan-bin,LI Yu-ru.Determination of S,S-enantiomer in (1R,2R)-(-)-1,2-cyclohexanediamine by GC[J].Progress in Pharmaceutical Sciences,2009,33(4):174-177.
Authors:ZHU Sheng-liang  SONG Xiao-guang  HAN Bin  ZHU Chuan-bin  LI Yu-ru
Institution:(Institute of Jiangsu Hengrui Medicine Co. Ltd., Lianyungang 222002, China)
Abstract: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.
Keywords:GC  ( 1R  2R)-(-)-1  2-cyclohexanediamine  S  S-enantiomer  pre-column derivatiza- tion  content determination
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