手性固定相HPLC法拆分苏氨酸和赖氨酸对映体  

Chiral separation of threonine and lysine enantiomers by HPLC

作　　者：朱晓伟[1] 秦书德[1] 刘健艺[1] 刘玉梅[2] 郭兴杰[1] 

机构地区：[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

出　　处：《西北药学杂志》2012年第1期26-28,共3页Northwest Pharmaceutical Journal

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。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.

关 键 词：苏氨酸 赖氨酸 对映体 手性固定相 高效液相色谱法 

分 类 号：R914[医药卫生—药物化学]