GC法测定琥珀酸普芦卡必利起始原料中的杂质  

Determination of impurities in the starting material of Prucalopride succinate by GC

作　　者：梅雪娇 闫翔宇 卢定强[3] 严相平 MEI Xuejiao;YAN Xiangyu;LU Dingqiang;YAN Xiangping(College of Biotechnology and Pharmaceutical Engineering,Nanjing Tech University,Nanjing,Jiangsu,211816 P.R.China;Pharmaceutical Department of Jiangsu Provincial Institute of Materia Media,Nanjing,Jiangsu,210009 P.R.China;School of Pharmaceutical Sciences,Nanjing Tech University,Nanjing,Jiangsu,211816 P.R.China;Nanjing Polytechnic Institute,Nanjing,Jiangsu,210044 P.R.China)

机构地区：[1]南京工业大学生物制药与工程学院,江苏南京211816 [2]江苏省药物研究所有限公司药学部,江苏南京210009 [3]南京工业大学药学院,江苏南京211816 [4]南京科技职业学院,江苏南京210044

出　　处：《华西药学杂志》2024年第1期72-74,共3页West China Journal of Pharmaceutical Sciences

摘　　要：目的用气相色谱法控制琥珀酸普芦卡必利起始原料1-(3-甲氧丙基)-4-哌啶胺中的杂质。方法采用CP-Sil8CB 5%苯基-95%二甲基聚硅氧烷毛细管柱(30 m×0.25 mm,0.5μm),以N_(2)为载气,气化室温度280℃,柱温150℃,检测器温度280℃,载气流量1.0 mL·min^(-1),分流比100∶1,进样量1μL。结果杂质A、B的线性范围分别为0.083~0.825、0.084~0.841 mg·mL^(-1),r^(2)分别为0.9971、0.9998,平均回收率分别为109.8%、102.9%,RSD分别为2.24%、2.03%。结论所用方法能有效地控制起始原料中的杂质A、B,可得到高纯度的琥珀酸普芦卡必利。OBJECTIVE To control the impurities in 1-(3-methoxypropyl)-4-piperidine from the starting material of Prucalopride succinate.METHODS The sample was analyzed by Gas chromatography using the CP-Sil8CB capillary column of(5%)phenyl-(95%)dimethyl polysiloxane(30 m×0.25 mm,0.5μm)as the analytical column.The carrier gas was N_(2),and the gasification chamber temperature was 280℃.The column temperature was 150℃with the detector temperature of 280℃,the carrier gas flow was 1.0 mL·min^(-1),the split ratio was 100∶1,and the injection volume was 1μL.RESULTS The linear range of impurity A was 0.083-0.825 mg·mL^(-1)(r^(2)=0.9971).The average recovery was 109.8%,RSD=2.24%.The linear range of impurity B was 0.08-0.841 mg·mL^(-1)(r^(2)=0.9998),and the average recovery was 102.9%,RSD=2.03%.CONCLUSION The method used can effectively control the impurities A and B in 1-(3-methoxypropyl)-4-piperidinamine to obtain high purity Prucalopride succinate.

关 键 词：琥珀酸普芦卡必利 1-(3-甲氧丙基)-4-哌啶胺 3-(4-氨基哌啶-1-基)-1-丙醇 1-丙基-4-哌啶胺 气相色谱法 杂质 吸附 质量控制 

分 类 号：R917[医药卫生—药物分析学]