GC测定盐酸帕洛诺司琼原料药中(S)-3-氨基-奎宁的含量

Determination of(S )-3-Aminoquinuclidine Content in Drug Substance of Palonosetron Hydrochloride by GC

目的:建立气相色谱法测定盐酸帕洛诺司琼原料药中(S)-3-氨基-奎宁含量的方法。方法:采用SE-30色谱柱(53 mm×60 m,5μm),起始温度100℃,维持5 min,再以20℃/min的速度升温至180℃,维持15 min,FID检测器。结果:(S)-3-氨基-奎宁线环性关系良好,相关系数为0.999 7,定量限为0.007 5 mg/m L,检测限为0.002 5 mg/m L,方法回收率为101.4%,RSD为3.2%,满足要求。结论:本法灵敏、可靠,可用于盐酸帕洛诺司琼原料药中(S)-3-氨基-奎宁的质量控制。

Objective ：To develop an GC method for determination of（S）-3-aminoquinuclidine content in drug substance of palonosetron hydrochloride. Methods ： A SE-30 column（53 mm × 60 m, 5 μm） was used at an initial temperature of 100 ℃ for 5 min, then the temperature increased at a rate of 20 ℃ / min to 180 ℃ and was maintained for 15 min. The detector used was FID. Results ： The calibration curve of（S）-3-aminoquinuclidine showed good linearity, with a correlation coefficient of 0.999 7. The limit of quantitatiion（LOQ） and limit of detection（LOD） of the method were 0.007 5 and 0.002 5 mg/m L respectively, while the recovery rate was 101. 4%,with a RSD of 3.2%, which met the relevant requirements. Conclusion ：The developed method was sensitive and reliable, which was applicable for the quality control of（S）-3-aminoquinuclidine in drug substance of palonosetron hydrochloride.