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目的建立2-[2-甲基-4-[4-[2-[4-(三氟甲基)苯基]嘧啶基]甲硫基]苯氧基]乙酸原料药中乙腈、1,4-二氧六环、四氢呋喃、乙酸乙酯、丙酮、乙醇和异丙醇7种有机溶剂残留量的气相色谱测定方法。方法采用DB-1(30 m×0.53 mm,5.00μm)毛细管色谱柱,氢火焰离子化检测器(FID),以氮气为载气,进样口温度160℃,检测器温度为250℃,柱温为程序升温;分流进样,外标法计算残留溶剂的含量。结果 7种有机溶剂均得到有效分离,在考察的浓度范围内,回收率及线性关系良好,且3批样品中有机溶剂残留量均符合规定。结论本方法操作简便,精密度好,准确可靠,适用于该原料中7种残留有机溶剂的同时测定。
Aim To establish a method for the determination of 2-methyl-4- [4- [2- [4- (trifluoromethyl) phenyl] pyrimidinyl] methylthio] phenoxy] Determination of Residues of Seven Kinds of Organic Solvents in Dioxane, Tetrahydrofuran, Ethyl Acetate, Acetone, Ethanol and Isopropanol by Gas Chromatography. Methods The capillary column with DB-1 (30 m × 0.53 mm, 5.00 μm) and the flame ionization detector (FID) were used with nitrogen as the carrier gas. The inlet temperature was 160 ℃ and the detector temperature was 250 ℃. Temperature for the program temperature; shunt injection, external standard method to calculate the residual solvent content. Results Seven kinds of organic solvents were effectively separated. The recoveries and linearities were good within the investigated concentration range, and the residues of organic solvents in the three batches of samples all met the requirements. Conclusion The method is simple, accurate, accurate and reliable. It is suitable for simultaneous determination of seven kinds of residual organic solvents in this raw material.