目的 建立同時測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種有機(jī)溶劑殘留量的頂空氣相色譜法。方法 采用Agilent DB-624（30 m×0.53 mm×3 μm）毛細(xì)管色譜柱；火焰離子化檢測器；進(jìn)樣口溫度200℃；檢測器溫度250℃；載氣為氮?dú)?；載氣體積流量為2.0 mL·min^-1；分流比為10：1；升溫程序：起始溫度40℃，保持6 min，以8℃·min^-1的速率升溫至90℃，保持2 min，再以20℃·min^-1的速率升溫至200℃，保持5 min；采用頂空進(jìn)樣方式，頂空加熱箱溫度80℃，樣品瓶平衡時間30 min。進(jìn)行系統(tǒng)適用性、檢測限（LOD）與定量限（LOQ）、線性關(guān)系和范圍、加樣回收率、精密度、穩(wěn)定性、耐用性考察。結(jié)果 注射用胸腺法新中5種殘留溶劑在各自線性濃度范圍內(nèi)與峰面積線性關(guān)系良好；平均加樣回收率在95.7%~106.3%；精密度、穩(wěn)定性、耐用性均符合要求。5批胸腺法新中均未檢出5種有機(jī)溶劑。結(jié)論 建立的頂空氣相色譜法操作簡單、靈敏度和準(zhǔn)確度高、重現(xiàn)性和耐用性好，可用于注射用胸腺法新中5種有機(jī)溶劑殘留量的測定。

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

四川省科技計劃項目：高端制劑共性關(guān)鍵技術(shù)研究與公共技術(shù)服務(wù)示范基地建設(shè)（2020YFS0570）