摘要
建立了反相高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定缬氨酸样品中杂质氨基酸含量的方法。采用Hypersil BDS C18色谱柱(4.6×250mm,5μm),以0.1%三氟乙酸乙腈溶液-0.1%三氟乙酸水溶液为流动相进行线性梯度洗脱,流速为0.8mL.min-1,在漂移管温度60℃,氮气流量1.5L.min-1的条件下,在25min内完成缬氨酸样品中杂质氨基酸的分离测定。在线性范围内,各组分进样质量的常用对数值与峰面积的常用对数值均呈良好的线性关系。精密度和重复性较好,样品的加样回收率为97.5%～98.0%。该方法检测速度快、检测过程简单方便、检测结果准确可信,可以作为缬氨酸样品中杂质氨基酸含量的检测方法,也为其他原料药中氨基酸的分析提供了参考。
An analytical method to determine amino acid impurities in valine samples was established by reversed-phase high performance liquid chromatography（HPLC） coupled with evaporative light-scattering detection（ELSD）.A hypersil BDS C18 column was used with the mobile phase of 0.1% trifluoroacetic acid acetonitrile solution-0.1% trifluoroacetic acid solution.Under the condition of solvent gradient elution,the detection was performed at the drift tube temperature of 60 ℃ and the nitrogen flow rate of 1.5 L/min.The flow rate was 0.8 mL/min.The amino acid impurities were separated in 25min.The calibration curves were showed good linearity in the linear range.The experimental results showed that the method had good precision and repeatability,the recovery was 97.5%～98.0%.The method was simple and rapid.The determined results were accurate and reliable.
出处
《化工技术与开发》
CAS
2011年第6期38-40,共3页
Technology & Development of Chemical Industry
关键词
反相高效液相色谱
蒸发光散射检测
氨基酸
缬氨酸
reversed-phase high performance liquid chromatography
evaporative light-scattering detection
amino acid
valine
作者简介
任洪发（1976-），男，湖北嘉鱼人，工程师，主要从事食品添加剂和医药原料药的合成研究及管理工作
