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目的:用毛细管气相色谱法建立新药Ⅰb原料中9种残留溶剂的测定方法。方法:采用DB-624毛细管柱(30.0 m×530μm,3.00μm),以氮气为载气,FID检测器,溶液直接分流进样,以正丁醇为内标,计算甲醇、乙醇、乙醚、二氯甲烷、正己烷、乙酸乙酯、甲苯和N,N-二甲基甲酰胺的含量;采用ECD检测器,通过外标法计算氯仿的含量。结果:在考察的浓度范围内,各溶剂均呈良好的线性关系(r>0.999 4)。平均回收率范围为97.1%~103.3%。结论:本方法稳定可靠,灵敏度高,结果准确,可用于新药Ⅰb原料中各有机残留溶剂的测定。
OBJECTIVE: To establish a method for the determination of nine residual solvents in new drug Ⅰb by capillary gas chromatography. Methods: DB-624 capillary column (30.0 m × 530μm, 3.00μm) was used to conduct direct injection of the solution with nitrogen as the carrier gas and FID detector. The n-butanol was used as the internal standard to calculate the concentration of methanol, ethanol, Methyl chloride, n-hexane, ethyl acetate, toluene, and N, N-dimethylformamide. The content of chloroform was calculated by an external standard method using an ECD detector. Results: The solvents showed a good linear relationship (r> 0.999 4) within the investigated concentration range. The average recovery ranged from 97.1% to 103.3%. Conclusion: The method is stable and reliable, with high sensitivity and accurate results. It can be used for the determination of organic residual solvents in new drug Ⅰb raw materials.