文章编号：1004－5422(2021)03－0237－05                                               DOI:10.3969/j.issn.1004-5422.2021.03.003

聂忠莉¹，王海龙¹，王晓玲²，高  华²，张  勇²，萧茂玲²

（1.成都大学  食品与生物工程学院，四川  成都  610106； 2.成都克莱蒙医药科技有限公司，四川  成都  610041）

摘  要：采用气相色谱法及残留溶剂测定法对他达拉非的残留溶剂进行测定.用6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的毛细管柱为色谱柱；柱温在50 ℃保持5min，再以30 ℃/min的速率升至240 ℃，维持5min；检测器为氢火焰离子化检测器，检测器温度为260 ℃，进样口温度为220 ℃，载气流速3.0mL/min，分流比10：1；进样体积1μL，记录色谱图.本方法可以有效、准确地检测出他达拉非的残留溶剂.
关键词：气相色谱法；残留溶剂测定法；异丙醇；乙腈；四氢呋喃；三乙胺
中图分类号：R927.2           文献标识码：A

Determination of Residual Solvent in Tadalafil by GC

NIE Zhongli¹,Wang Hailong¹,WANG Xiaoling²,GAO Hua²，ZHANG Yong²，XIAO Maoling²

(1.School of Food and Biological Engineering,Chengdu University,Chengdu 610106,China; 

2. Chengdu Climb Pharmaceutical Technology Co.,Ltd.,Chengdu 610041,China）

Abstract：The paper aims to determine the residual solvent in tadalafil by gas chromatography and residual solvent determination.The chromatographic column consists of 6% propyl phenyl-94% dimethyl polysiloxane which were utilized as fixed liquid capillary column;the whole process lasted for 5 minutes with the column temperature at 50 ℃ before it rose at a rate from about 30 ℃ / min to 240 ℃,which lasted for 5 minutes; the detector for hydrogen flame was an ionization detector; the test temperature was 260 ℃; the sample temperature was 220 ℃; the carrier gas flow rate was 3.0 mL/min,and the diversion ratio was 10∶1. The sample introduction volume was 1μL and the chromatogram was recorded. It is concluded that this method can effectively detect residual solvents in tadalafil.
Key words：gas chromatography; residual solvent determination method; isopropanol; acetonitrile; tetrahydrofuran; triethylamine