气相色谱法测定环戊基肼盐酸盐的含量  

Content Determination of Cyclopentylhydrazine Hydrochloride by Gas Chromatography

作　　者：钱日彬 王健松 叶海鸿 鲍颖霞 QIAN Ribin;WANG Jiansong;YE Haihong;BAO Yingxia(Guangzhou BaiYunShan Pharmaceutical Holdings Co.,Ltd.,Guangzhou Baiyunshan Pharmaceutical General Factory,Guangzhou,Guangdong 510515,China;Key Laboratory of Key Technology Research on Chemical Raw Materials and Preparations of Guangdong Province,Guangzhou,Guangdong 510515,China)

机构地区：[1]广州白云山医药集团股份有限公司白云山制药总厂,广东广州510515 [2]广东省化学药原料与制剂关键技术研究重点实验室,广东广州510515

出　　处：《今日药学》2022年第6期448-452,461,共6页Pharmacy Today

基　　金：国家科技重大专项(民口)课题(2019ZX09301-104);广东省省级科技计划项目(2021A0505080010)。

摘　　要：目的建立气相色谱法测定环戊基肼盐酸盐的含量。方法采用气相色谱法,色谱柱为InterCap for Amines毛细管色谱柱(30 m×0.32 mm,0.25μm),FID检测器,进样口温度为200℃,检测器温度为280℃,柱温采用程序升温,初始柱温为60℃,保持4 min,以10℃·min^(-1)的速率升温至140℃,再以6℃·min^(-1)的速率升温至250℃,保持5 min,载气为氮气,流速为1.5 mL·min^(-1),分流比5∶1,进样量为1μL。结果分离度良好,空白溶剂无干扰。环戊基肼盐酸盐进样浓度在5.11~12085.00μg·mL^(-1)具有良好的线性关系(r=0.9999),定量限5.38μg·mL^(-1),检测限为2.66μg·mL^(-1),平均回收率(n=9)为101.0%。结论本方法操作简便、灵敏度高、准确度和重复性好,可用于环戊基肼盐酸盐含量的测定。OBJECTIVE To establish a gas chromatography(GC)method for the determining the content of cyclopentylhydrazine hydrochloride.METHODS The GC was performed on an InterCap for Amines capillary column(30 m×0.32 mm,0.25μm)with a flame ionization detector(FID).The injector temperature was 200℃,and detector temperature was set at 280℃.The column temperature was set as follows:60℃ for 4 min,increased to 140℃ at a rate of 10℃·min^(-1),then at 6℃·min^(-1) to 250℃,held for5 min.The carrying gas was nitrogen and the flow rate of gas was 1.5 mL·min^(-1).The injection spilt ratio was 5∶1.And the injection volume was 1μL.RESULTS The resolution of the cyclopentylhydrazine hydrochloride to be tested was good,and the blank solvent had no interference.The calibration curve of cyclopentylhydrazine hydrochloride was in good linear correlation in the concentration rang of 5.11-12085.00μg·mL^(-1)(r=0.9999).The limit of quantification was 5.38μg·mL^(-1),The detection limit was 2.66μg·mL^(-1).The mean recovery(n=9)was 101.0%.CONCLUSION This method is simple,sensitive,accurate and reproducible.It can be used for determination of cyclopentylhydrazine hydrochloride.

关 键 词：气相色谱法 环戊基肼盐酸盐 含量测定 

分 类 号：R917[医药卫生—药物分析学]