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目的建立顶空进样气相色谱法测定恩格列净原料药中10种溶剂的残留量,以期为恩格列净原料药的质量控制提供试验依据。方法采用顶空气相色谱法测定;毛细管色谱柱为Aglient DB-624柱(25 m×0.53 mm,3.0μm);程序升温;FID检测器;氮气为载气;流速为1.0 m L·min-1;顶空平衡温度为80℃;平衡时间为20 min;用外标法计算甲醇、乙腈、二氯甲烷、环己烷、四氢呋喃、乙醇、乙醚、叔丁基甲醚、乙酸乙酯和乙酸共10种残留溶剂的含量。结果在本色谱条件下10种残留溶剂在各自的质量浓度范围内均具有良好的线性关系,平均回收率为90.45%~102.45%,重复性RSD≤2%(n=6)。结论本方法适用于恩格列净原料药中溶剂残留量的检查。
OBJECTIVE To establish a headspace gas chromatographic method for the determination of 10 solvents in the encephalitozuron raw material for the purpose of providing experimental evidence for the quality control of enzapine. The method was carried out by headspace gas chromatography. The capillary column was Aglient DB-624 column (25 m × 0.53 mm, 3.0 μm); the temperature was programmed; FID detector; nitrogen was the carrier gas; the flow rate was 1.0 m L · min -1 ; Equilibrium temperature of headspace is 80 ℃; equilibrium time is 20 min; total 10 methanol, acetonitrile, methylene chloride, cyclohexane, tetrahydrofuran, ethanol, ether, tert-butyl methyl ether, ethyl acetate and acetic acid Residual solvent content. Results Under the chromatographic conditions, the 10 residual solvents showed a good linearity within the range of their respective mass concentrations. The average recoveries ranged from 90.45% to 102.45% and the repeatability RSD ≤ 2% (n = 6). Conclusion This method is suitable for the determination of solvent residues in enqling net medicine.