GC测定盐酸普拉克索中三乙胺残留量

目的 建立盐酸普拉克索原料中三乙胺残留量测定方法。方法 采用顶空气相色谱法,FID检测器,以100%二甲基聚硅氧烷为固定液的Agilent DB-1毛细管柱（30 m×0.530 mm,3.00μm）,载气为氮气,流速：4.0 mL.min 1,进样口温度为200℃,检测器温度为250℃,柱温采用程序升温,初始温度为50℃,保持5 min,然后以10℃.min 1升至150℃再以40℃.min 1升至220℃,保持5 min;顶空条件为80℃平衡30 min,以20%氢氧化钠溶液为溶剂配制对照品溶液及样品溶液,采用外标法定量。结果 三乙胺浓度在0.317∽12.68μg.mL 1内有良好的线性关系（r=0.999 8）,平均回收率为97.9%（n=9）,RSD为4.18%（n=9）。结论 本方法准确、可靠、灵敏度高,适用于盐酸普拉克索中三乙胺的残留量检测。同时该方法为测定盐酸、醋酸盐类药物中的三乙胺残留提供了一个思路。

Determination of Triethylamine in Pramipexole Hydrochloride by Headspace GC

OBJECTIVE To determine the triethylamine in pramipexole hydrochloride by GC. METHODS The residual triethylamine was determined by HS-GC with Agilent-INNOWAX capillary column（30 m×0.32 mm, 0.5μm） and FID detector. The carrier gas was nitrogen and the flow rate was 4.0 mL-min-1. The temperature of the injection port was maintaining at 250 ℃ and the same of detector. The oven introduced sequential increasing of temperature programing. The initial column temperature was 50℃, then raised the temperature to 150℃ at a rate of 10 ℃＇min-1, and maintained it at 150 ℃ for 5 min, then raised the temperature to 220℃ at a rate of 40 ℃.min-1, and maintained it for 5 min. The headspace oven was set at a temperature of 80 ℃ for 30 rain. The solvent was 20% sodium hydroxide solution. The triethylamine was quantified external standard. RESULTS The calibration shows a good linearity with the range of 0.317-12.68μg.mL-1 for triethylamine. The average recovery was 97.9%（n=9）. The precision was 4.18%（n=9）. CONCLUSION This method is accurate, reliable and sensitive for the determination of the residual quantity of triethylamine in pramipexole hydrochloride.