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.
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)
出处
《山东化工》
CAS
2022年第7期105-107,共3页
Shandong Chemical Industry
关键词
气相色谱法
1-叔丁氧羰基哌嗪
哌嗪
方法学
GC
1-(tert-butoxycarbonyl)piperazine
piperazine
analytical validation
