气相色谱法测定1-叔丁氧羰基哌嗪中哌嗪的方法学研究  

GC Analysis and Methodology Research for Piperazine in 1-(Tert-Butoxycarbonyl)Piperazine

作　　者：伍鸣亮 张运海 曾海金 罗恒真 Wu Mingliang;Zhang Yunhai;Zeng Haijin;Luo Hengzhen(Jiangxi Qingfeng Pharmaceutical Co.,Ltd.,Ganzhou 341000,China)

机构地区：[1]江西青峰药业有限公司,江西赣州341000

出　　处：《山东化工》2022年第7期105-107,共3页Shandong Chemical Industry

摘　　要：建立气相色谱法测定1-叔丁氧羰基哌嗪中的哌嗪,该方法使用非极性固定相的气相色谱柱(Agilent CP-Volamine 30 m×0.32 mm)。起始温度为80℃,保持2 min,以20℃/min的速率升温至200℃并保持6 min;检测器温度为300℃;进样口温度为180℃;载气流速为4.0 mL/min。进样体积1μL。哌嗪的定量限为3.2μg/mL,在3.2~80μg/mL的线性函数关系较好,平均回收率为100.94%,回收率RSD为1.3%。本方法的专属性和检测准确度均较好,检测灵敏度较高,可用于1-叔丁氧羰基哌嗪的质量控制。A GC method has been established for detecting the piperazine in 1-(tert-butoxycarbonyl)piperazine.A non-polar stationary phase gas chromatography column(Agilent CP-Volamine 30 m×0.32 mm)was used.Maintain the column temperature at 80℃for 2 min,than raise temperature at a rate of 20℃/min to 200℃and maintain for 6 min;the temperature of detector is 300℃;the temperature of injetion port is180℃;the flow rate of the carrier gas is 4.0 mL/min.The injection volume is 1μL.The limit of piperazine was 3.2μg/mL,the method was linear from 3.2μg/mL to 80μg/mL,the accuracy was similar with a mean(RSD)ratio of 100.94%(1.3%).The method is specific,accuracy and sensitive,and can be used for the quality control of 1-(tert-butoxycarbonyl)piperazine.

关 键 词：气相色谱法 1-叔丁氧羰基哌嗪 哌嗪 方法学 

分 类 号：O657.7[理学—分析化学]