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目的建立TM-2中9种有机溶剂残留量测定法。方法采用气相色谱法,色谱柱为DB-624(30 m×530μm,3μm)毛细管柱,程序升温,检测器为FID,载气为氮气;采用顶空进样法,平衡温度为115℃,平衡时间为20 min。结果甲醇、乙腈、二氯甲烷、叔丁醇、正己烷、乙酸乙酯、四氢呋喃、三乙胺及吡啶线性关系良好(r≥0.992 9),平均回收率为89.9%~102.4%(RSD=3.6%),检测限分别为0.28、0.30、0.53、0.22、0.03、0.07、0.05、0.15、0.15 mg·L-1。结论本方法可用于TM-2原料药中残留溶剂的检查。
Objective To establish a method for the determination of nine organic solvents in TM-2. Methods The column was DB-624 (30 m × 530μm, 3μm) capillary column. The temperature was programmed, the detector was FID, and the carrier gas was nitrogen. The headspace sampling method was used. The equilibrium temperature was 115 ℃ and the equilibrium The time is 20 min. The results showed good linearity (r≥0.992 9) for methanol, acetonitrile, dichloromethane, t-butanol, n-hexane, ethyl acetate, tetrahydrofuran, triethylamine and pyridine. The average recoveries were 89.9% ~ 102.4% %), The detection limits were 0.28,0.30,0.53,0.22,0.03,0.07,0.05,0.15,0.15 mg · L-1. Conclusion This method can be used for the determination of residual solvents in TM-2 APIs.