GC法测定高哌嗪中乙二胺和哌嗪的残留量  

Determination of ethylenediamine and piperazine residues in homopiperazine by GC

作　　者：甘冬彦 杨建玲 杨晓芸 陈云建 GAN Dongyan;YANG Jianling;YANG Xiaoyun;CHEN Yunjian(Dali University,Dali 671000,China;KPC Pharmaceuticals,Inc.,Kunming 650100,China)

机构地区：[1]大理大学,云南大理671000 [2]昆药集团股份有限公司,云南昆明650100

出　　处：《药物评价研究》2020年第6期1071-1074,共4页Drug Evaluation Research

摘　　要：目的建立气相色谱法(GC)测定高哌嗪中杂质残留乙二胺和哌嗪。方法采用GC法,色谱柱为CP-sil8 CB(30 m×0.25 mm×0.50μm);进样口温度240℃;升温程序:60℃保持1 min,以5℃/min的速率升温至110℃,再以40℃/min的速率升温至200℃,保持3 min;检测器为氢火焰离子化检测器(FID),检测器温度为250℃;载气为氮气;分流比为2∶1;进样方式为直接进样,进样量1μL;体积流量:1 mL/min。结果高哌嗪中乙二胺杂质和哌嗪杂质与主成分间均能有效分离,线性范围分别为20.2~161.7μg/mL(r=0.9998),20.4~163.6μg/mL(r=0.9999)。重复性和精密度的RSD值均在规定范围内。结论该方法适用于高哌嗪中乙二胺和哌嗪杂质的准确测定和质量控制。Objective A GC method was established to determine the residual impurities of ethylenediamine and piperazine in homopiperazine.Methods Gas chromatography was applied to this study.The determination was carried out on CP-sil8 CB(30 m×0.25 mm×0.50μm).Injection temperature was 240℃.Temperature rise procedure was kept at 60℃for 1 min,then the temperature was raised to 110℃at the rate of 5℃/min.And the temperature was raised to 200℃at the rate of 40℃/min for 3 min.The detector was FID,and the detector temperature was 250℃.The carrier gas was nitrogen,the split ratio was 2:1.The injection volume was 1μL,the flow rate was 1 mL/min.Results Ethylenediamine impurity and piperazine impurity in homopiperazine can be separated from the principal component effectively.The linear range was 20.2—161.7μg/mL(r=0.9998),and 20.4—163.6μg/mL(r=0.9999),respectively.The RSD values of repeatability and precision were within the specified range.Conclusion The method is simple,accurate and reliable,and has good specificity,and can be used for quality control of homopiperazine.

关 键 词：高哌嗪 乙二胺 哌嗪 气相色谱法 质量控制 

分 类 号：R927.2[医药卫生—药学]