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手性固定相HPLC法拆分苏氨酸和赖氨酸对映体
引用本文:朱晓伟,秦书德,刘健艺,刘玉梅,郭兴杰. 手性固定相HPLC法拆分苏氨酸和赖氨酸对映体[J]. 西北药学杂志, 2012, 27(1): 26-28. DOI: 10.3969/j.issn.1004-2407.2012.01.012
作者姓名:朱晓伟  秦书德  刘健艺  刘玉梅  郭兴杰
作者单位:1. 沈阳药科大学,沈阳,110016
2. 锦州九泰药业有限责任公司,锦州,121012
摘    要:目的建立了柱前衍生结合手性固定相HPLC法拆分了苏氨酸和赖氨酸2种氨基酸对映体。方法利用4-氯-7-硝基-2,1,3-苯并噁二唑(NBD-Cl)柱前衍生,采用Sumichiral OA-2500S色谱柱,以甲醇-乙腈(60∶40,含5mmol.L-1柠檬酸)为流动相,检测波长为470nm。结果应用该法检查L-氨基酸原料药中的D-型异构体,D-苏氨酸和D-赖氨酸在2.0~16.0μg.mL-1质量浓度范围内线性关系良好,回收率均为101.0%,RSD分别为1.7%和0.37%。结论在最佳色谱条件下,2种氨基酸对映体均达到了基线分离。建立的对映体杂质检查方法灵敏度高,重复性好。

关 键 词:苏氨酸  赖氨酸  对映体  手性固定相  高效液相色谱法

Chiral separation of threonine and lysine enantiomers by HPLC
ZHU Xiaowei,QIN Shude,LIU Jianyi,LIU Yumei,GUO Xingjie. Chiral separation of threonine and lysine enantiomers by HPLC[J]. Northwest Pharmaceutical Journal, 2012, 27(1): 26-28. DOI: 10.3969/j.issn.1004-2407.2012.01.012
Authors:ZHU Xiaowei  QIN Shude  LIU Jianyi  LIU Yumei  GUO Xingjie
Affiliation:1(1.Shenyang Pharmaceutical University,Shenyang 110016,China;2.Jinzhou Jiutai Pharmaceutical Limited-liability Company,Jinzhou 121012,China)
Abstract:Objective To establish chiral stationary phases(CSPs) combining with pre-column derivation method for the chiral separation of threonine(Thr) and lysine(Lys).Method The enantiomers of threonine and lysine were derivatized with reagent 4-chloro-7-nitro-2,1,3-benzoxadiazole(NBD-Cl).The diastereoisomers produced were separated on a Sumichiral OA-2500S CSP column with a mobile phase consisting of methanol(including 5 mmol·L-1 citric acid)-acetonitrile(60∶40) and wavelength was set at 470 nm.Results The calibration curves of D-threonine,and D-lysine were linear in the concentration range of 2.0-16.9 μg·mL-1.The average recoveries of D-threonine and D-lysine were 101.0%,with RSD of 1.7%and 0.37%,respectively.Conclusions Under the optimized chromatographic conditions,baseline separations of these amino acid enantiomers were obtained.The method is sensitive and reproducible.
Keywords:threonine  lysine  enantiomeric  CSPs  HPLC
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