气相色谱法测定盐酸比生群中溶剂残留量

Determination of organic residual solvents inbisantrene hydrochloride by gas chromatography

目的 :测定盐酸比生群原料中残留有机溶剂甲醇、1,4 -二氧六环和甲苯的含量。方法 :采用气相色谱法 ,氢火焰离子化检测器 (FID) ,以水为溶剂 ,异丙醇为内标 ,采用 2 m不锈钢填充柱 ,80 / 10 0目 ,Carbopack担体 ,上附 0 .2 %Carbowax 15 0 0固定液 ;柱温 12 0 o C维持 4分钟 ,以 70 o C/ min的速率升温至 15 0℃ ,维持 7.5分钟 ;气化室温度 :15 0 o C;检测器温度 :180 o C(FID) ;载气 :氮气 ;柱前压 :33Psi。实现了各组分的基线分离。结果 :3批盐酸比生群原料中 3种有机溶剂残留量均符合规定。结论 :经方法学试验验证 ,该方法灵敏、准确、可信 ,适用于本品有机溶剂残留量的测定。

Object: To determine the content of the residual of organic volatile solvents including methanol, 1,4-dioxane and toluene in bisantrene hydrochloride raw material. Methods: A GC method with FID detection was used. Dissolved in water, 2μL of the solution was injected on a Carbopack column, using nitrogen as carrier gas and isopropanol as internal standard. The column inlet pressure was 33Psi, range was 2 and attenuation was 2. The initial temperature was kept at 120℃ for 4 min, then the temperature was raised to 150℃ at the rate of 70℃·min1, and subsequently sustained for 7.5 min. The injection port and detector temperature were 150℃ and 180℃ respectively. Under this condition, methanol, 1,4-dioxane, toluene and the internal standard isopropanol were separated thoroughly Results: Three batches of samples were analyzed using the above method. None of the three samples were found to exceed the limit. Conclusion: After validation, the method was proved to be accurate, sensitive and reliable. It is quite suitable to be used in the analysis of the organic volatile solvent in bisantrene hydrochloride.