目的 建立同时测定注射用胸腺法新中乙腈、二氯甲烷、醋酸乙酯、苯和苯甲醚5种有机溶剂残留量的顶空气相色谱法。方法 采用Agilent DB-624（30 m×0.53 mm×3 μm）毛细管色谱柱；火焰离子化检测器；进样口温度200℃；检测器温度250℃；载气为氮气；载气体积流量为2.0 mL·min^-1；分流比为10：1；升温程序：起始温度40℃，保持6 min，以8℃·min^-1的速率升温至90℃，保持2 min，再以20℃·min^-1的速率升温至200℃，保持5 min；采用顶空进样方式，顶空加热箱温度80℃，样品瓶平衡时间30 min。进行系统适用性、检测限（LOD）与定量限（LOQ）、线性关系和范围、加样回收率、精密度、稳定性、耐用性考察。结果 注射用胸腺法新中5种残留溶剂在各自线性浓度范围内与峰面积线性关系良好；平均加样回收率在95.7%~106.3%；精密度、稳定性、耐用性均符合要求。5批胸腺法新中均未检出5种有机溶剂。结论 建立的顶空气相色谱法操作简单、灵敏度和准确度高、重现性和耐用性好，可用于注射用胸腺法新中5种有机溶剂残留量的测定。

Objective To establish HS-GC method to simultaneously determine the residues of five organic solvents (acetonitrile, dichloromethane, ethyl acetate, benzene, and anisole) in thymalfasin for injection. Methods The determination was performed on Agilent DB-624 capillary column (30 m×0.53 mm×3 μm) with temperature programming by FID. The inlet temperature was 200℃ and the detector temperature was 250℃. The carrier gas was nitrogen, and the carrier gas flow rate was 2 mL·min^-1. The column temperature started at 40℃ for 6 min, and then at 8℃·min^-1 to 90℃ for 2 min, followed by 20℃·min^-1 to 200℃ for 5 min. The temperature of HS heating box was 80℃ and the equilibrium time of sample bottle was 30 min. Results The five residual solvents in thymalfasin for injection had a good linear relationship in their concentration ranges (r > 0.999). The average recovery was 95.7%-106.3%. Precision, stability and durability all meet the requirements. Conclusion The method is simple, sensitive, accurate, reproducible and durable, and can be used to determine the residues of five organic solvents in thymalfasin for injection.

R917

四川省科技计划项目：高端制剂共性关键技术研究与公共技术服务示范基地建设（2020YFS0570）