HPLC法测定L-脯氨酰胺中手性异构体杂质  

Determination of Chiral Isomer Impurities in L-Proline Amide by HPLC

作　　者：黄祥元 蒋艾青[1] Huang Xiang-yuan;Jiang Ai-qing

机构地区：[1]永州职业技术学院

出　　处：《化工设计通讯》2019年第12期63-64,共2页Chemical Engineering Design Communications

摘　　要：目的 :建立高效液相色谱法(HPLC)测定L-脯氨酰胺中手性异构体杂质D-脯氨酰胺的方法。方法 :色谱柱,CHIRALPAK@IC手性色谱柱(250mm×4.6mm,5μm),以正己烷-乙醇-二乙胺(70∶30∶0.1)为流动相,流速为1mL/min,检测波长为220nm,柱温为35℃,进样量为20μL。结果 :D-脯氨酰胺浓度在4.0~202.2μg/mL,其浓度与峰面积成良好的线性关系,线性回归方程为y=1 251.8x-6 076.1,r=0.999 5;D-脯氨酰胺的检测限、定量限分别为10ng、30ng;平均加样回收率为99.6%,RSD为0.8%。结论 :本方法简单,灵敏,重现性好,准确度高,可用于L-脯氨酰胺中手性异构体杂质的控制。Objective :To establish a high performance liquid chromatography(HPLC)method for the determination of chiral isomer impurity D-proline in L-proline.Method :Chromatographic column :CHIRALPAK @ IC chiral column(250 mm × 4.6 mm,5μm),n-hexane-ethanol-diethylamine(70 ∶ 30 ∶ 0.1)as mobile phase,flow rate is 1 ml/min,detection wavelength 220 nm,column temperature is 35℃,and injection volume is 20 ul.Results:The concentration of D-prolineamide was in the range of 4.0-202.2 ug/ml,and its concentration had a good linear relationship with the peak area.The linear regression equation was y=1251.8 x-6076.1,r=0.9995;The detection limit and quantitation limit were 10 ng and 30 ng,respectively;the average sample recovery was 99.6%,and the RSD was 0.8%.Conclusion :This method is simple,sensitive,reproducible,and accurate.It can be used for the control of chiral isomer impurities in L-proline amide.

关 键 词：L-脯氨酰胺 D-脯氨酰胺 异构体 HPLC 

分 类 号：TQ460.7[化学工程—制药化工]