柱前衍生RP-HPLC-DAD法测定氨茶碱片及注射液中乙二胺的含量  

Determination of ethylenediamine in aminophylline tablets and aminophylline injection by RP-HPLC-DAD with pre-column derivatization

作　　者：吴月霞 杨本霞[1] 陈杰[1] WU Yuexia;YANG Benxia;CHEN Jie(Henan Institute for Food and Drug Control,Zhengzhou 450018,China)

机构地区：[1]河南省食品药品检验所,郑州450018

出　　处：《中国药品标准》2022年第4期381-385,共5页Drug Standards of China

摘　　要：目的:建立柱前衍生反相高效液相色谱法测定氨茶碱片及氨茶碱注射液中乙二胺的含量测定方法。方法:采用Agilent 5 TC-C_(18)(2)色谱柱(4.6 mm×250 mm,5μm),水(A)-乙腈(B)为流动相,梯度洗脱(0~12 min,60%→45%A,12~13.2 min,45%→25%A,13.2~18 min,25%→60%A,18~20 min,60%→60%A),柱温30℃,流速1.0 mL·mL^(-1),紫外检测波长为228 nm,进样量10μL。结果:主成分与其他成分能达到良好的分离;乙二胺的线性范围为1.076~10.757μg·mL^(-1),线性方程为Y=228.0731 X+24.1775(r=0.9999);理论板数大于50000,各相邻峰分离度均大于3,检测限为3.404 ng·mL^(-1),定量限为11.346 ng·mL^(-1);片剂的平均加标回收率为100.95%,RSD为0.34%(n=9);注射剂的平均加标回收率为100.45%,RSD为0.21%(n=9)。3批氨茶碱片剂中乙二胺的含量测定结果分别为16.7%、16.9%、16.4%;3批注射剂中乙二胺的平均含量分别为16.9%、16.8%、16.6%。结论:该法可用于氨茶碱片及氨茶碱注射液中乙二胺的质量控制。Objective:To establish a method for the determination of ethylenediamine in aminophylline tablets and aminophylline injection by RP-HPLC with pre-column derivatization.Methods:The analysis was performed on an Agilent 5 TC-C_(18)(2)column(4.6 mm×250 mm,5μm)at 30℃ using gradient elution of water(A)and acetonitrile(B)delivered at a flow rate of 1.0 mL·mL^(-1).The gradient elution was:0-12 min,60%→45%A;12-13.2 min,45%→25%A;13.2-18 min,25%→60%A;18-20 min,60%→60%A.The UV detection wavelength was 228 nm,and the sample size was 10μL.Results:The principal component and other components were well separated.The linear equation of ethylenediamine was Y=228.0731 X+24.1775(r=0.9999)in the range of 1.076-10.757μg·mL^(-1).The number of theoretical plates was greater than 50000,the resolution of each adjacent peak was greater than 3,the detection limit was 3.404 ng·mL^(-1),and the limit of quantification was 11.346 ng·mL^(-1).The average recovery was 100.95% with RSD of 0.34%(n=9).The average recovery was 100.45% with RSD of 0.21%(n=9).The content determination results of ethylenediamine in 3 batches of aminophylline tablets were 16.7%,16.9% and 16.4%,respectively.The average contents of ethylenediamine in 3 batches of aminophylline injection samples were 16.9%,16.8% and 16.6%,respectively.Conclusion:The method can be used for the quality control of ethylenediamine in aminophylline tablets and aminophylline injection.

关 键 词：柱前衍生化 氨茶碱片剂 氨茶碱注射剂 乙二胺 对甲苯磺酰氯 

分 类 号：R921.2[医药卫生—药学]