甘氨酸-谷氨酸和甘氨酸-酪氨酸中有机溶剂残留量检测

Determination of residual organic solvents in Glycine-Glutamic acid and Glycine-Tyrosine by GC

目的建立甘氨酸-谷氨酸和甘氨酸-酪氨酸原料药中有机溶剂甲苯和乙醇的测定方法。方法采用溶液直接进样气相色谱法,PEG-20M(30m×0.53mmI.D.Xlgm)石英毛细管柱,柱温70℃,载气为氮气,氢火焰离子化检测器,气化室温度180℃,检测器温度200℃。结果甲苯在9～138ppm.mL-1,乙醇在50～750ppm.mL-1范围内线性关系良好,相关系数分别为0.9996和0.9999,进样精密度的RSD分别为1.5%和1.1%。各组分实现了各组分的基线分离,测定3批甘氨酸-谷氨酸和甘氨酸-酪氨酸原料中有机溶剂残留量均符合规定。结论所建立方法灵敏、准确,可适用于甘氨酸-谷氨酸和甘氨酸-酪氨酸原料中有机溶剂残留量的测定。

OBJECTIVE To establish a method for the determination of residual organic solvents in Glycine-Glutamic acid and Glycine-Tyrosine raw material by the use of GC. METHODS The GC determination was performed on a glass column which was packed PEG-20M with FID detection. The injection port and detector temperature were 180℃ and 200℃, respectively. RESULTS Under experiment condition, Methylbenzene has good linear relationship between 9-138ppm·mL^- 1, RSD% of middle precision： 1.5 %. Ethanol has good linear relationship between 50- 750ppm·mL^-1, RSD% of middle precision： 1.1%. Every component was separated thoroughly. Three batches of samples were analyzed by the method. None of residual organic solvent was found to exceed quality limit. CONCLUSION The method is proved to be accurate and sensitive. It is suitable for the analysis of the residual organic solvents in Glycine-Glutamic acid and Glycine-Tyrosine raw material.