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
梅雪娇 1闫翔宇 2卢定强 3严相平4
作者信息
- 1. 南京工业大学生物制药与工程学院,江苏南京 211816;江苏省药物研究所有限公司药学部,江苏南京 210009
- 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
- 折叠
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-Si18CB5％苯基-95％二甲基聚硅氧烷毛细管柱(30 m×0.25 mm,0.5 μm),以N2为载气,气化室温度280℃,柱温150℃,检测器温度280 ℃,载气流量1.0mL·min-1,分流比100:1,进样量1 μL.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,r2 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.
Abstract
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,0.5 µm)as the analytical column.The carrier gas was N2,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 1 μL.RESULTS The linear range of impurity A was 0.083-0.825 mg·mL-1(r2=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(r2=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Key words
Prucalopride succinate/1-(3-Methoxypropyl)-4-piperidinamine/3-(4-Aminopiperidin-1-yl)propan-1-ol/1-Propylpiperidin-4-amine/GC/Impurities/Adsorption/Quality control引用本文复制引用
出版年
2024
NETL
NSTL
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