气相色谱法测定乙酸阿比特龙中1,1,3,3-四甲基胍  

Determination of 1,1,3,3-tetramethylguanidine in abiraterone acetate by gas chromatography

作　　者：宋小飞 王红芳 张辉 申晓婷 柴青叶 游蓉丽 SONG Xiaofei;WANG Hongfang;ZHANG Hui;SHEN Xiaoting;CHAI Qingye;YOU Rongi(Shanxi Zhendong Pharmaceutical Co.,Ltd.,Changzhi 046000,China)

机构地区：[1]山西振东制药股份有限公司,山西长治046000

出　　处：《化学分析计量》2023年第6期61-64,84,共5页Chemical Analysis And Meterage

摘　　要：建立气相色谱测定乙酸阿比特龙原料药中1,1,3,3-四甲基胍的方法。选择乙酸乙酯为溶剂溶解样品,以安捷伦CP-Volamine毛细管柱(30 m×0.32 mm,0.45μm)作为分离色谱柱,采用氢火焰离子化检测器(FID)进行检测,外标法定量分析。1,1,3,3-四甲基胍的质量浓度在10.22~204.38μg/mL范围内与色谱峰面积线性关系良好,相关系数为0.9994,定量限为10.22μg/mL。样品加标回收率为97.9%~113.7%,9份样品测定结果的相对标准偏差为5.0%。该方法操作简单,可用于乙酸阿比特龙原料中1,1,3,3-四甲基胍的测定。A method for the determination of 1,1,3,3-tetramethylguanidine in abiraterone acetate API(Active Pharmaceutical Ingredient)by gas chromatography was established.Ethyl acetate was selected as the solvent to dissolve the sample,the Agilent CP-Volamine capillary column(30 m×0.32 mm,0.45μm)was used as the chromatographic column,the flame ionization detector(FID)was used for detection,and the external standard method was used for quantification.The mass concentration of 1,1,3,3-tetramethylguanidine had a good linear relationship with the chromatographic peak area in the range of 10.22-204.38μg/mL,the correlation coefficient was 0.9994,and the limit of quantification was 10.22μg/mL.The recoveries of the samples were 97.9%-113.7%,and the relative standard deviation of the 9 samples was 5.0%.The method is simple,and it can be used for the determination of 1,1,3,3-tetramethylguanidine in the raw material of abiraterone acetate.

关 键 词：气相色谱法 乙酸阿比特龙 1 1 3 3-四甲基胍 

分 类 号：O657.7[理学—分析化学]