GC测定盐酸普拉克索中三乙胺残留量

Determination of Triethylamine in Pramipexole Hydrochloride by Headspace GC

关键词:  顶空气相色谱法  盐酸普拉克索  三乙胺

Key words:  headspace capillary GC  pramipexole hydrochloride  triethylamine

摘要:

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，3.00 μm)，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0.317~12.68 μg·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。

Abstract:

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, 0.5 μm) 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 min. 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?12.68 μg·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.