GC测定盐酸普拉克索中三乙胺残留量.PDF

GC 测定盐酸普拉克索中三乙胺残留量  李炎，邹剑，刘峰，李睿( 四川省食品药品检验检测院，成都 610097) 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 1 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 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。 关键词：顶空气相色谱法；盐酸普拉克索；三乙胺 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2014)07-0863-03 DOI: 10.13748/ki.issn1007-7693.2014.07.024 Determination of Triethylamine in Pramipexole Hydrochloride by Headspace GC LI Yan, ZOU Jian, LIU Feng, LI Rui(Sichuan Institute for Food and Drug Control, Chengdu 610097, China) 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 ext