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目的:建立同时测定生血宁片中7种残留溶剂(丙酮、2,3-二甲基戊烷、3-甲基己烷、正庚烷、2,2-二甲基己烷、邻二甲苯、2,4,6-三甲基吡啶)的方法。方法:采用顶空毛细管柱气相色谱法,色谱柱为DB-5MS毛细管柱(30 m×0.25 mm,0.25μm),程序升温;载气为氮气,流速为2.5 ml·min~(-1);进样口温度200℃;检测器为FID检测器,检测器温度为250℃;顶空进样,顶空瓶平衡温度为95℃,平衡时间为30 min。以DMF为溶剂,用外标法测定7种残留溶剂的量,进样量为1 ml。结果:在该色谱条件下,7种有机溶剂均能得到良好分离,各溶剂在所考察的质量浓度范围内与峰面积线性关系良好(r≥0.994 4),平均加样回收率为98.72%~99.91%(RSD为0.14%~0.71%)(n=9)。结论:该方法简便快速,灵敏度高,可用于生血宁片中有机溶剂残留量的同时测定。
OBJECTIVE: To establish a method for the simultaneous determination of seven residual solvents (acetone, 2,3-dimethylpentane, 3-methylhexane, n-heptane, 2,2-dimethylhexane, , 2,4,6-trimethylpyridine). Methods: The capillary column was a capillary column (30 m × 0.25 mm, 0.25 μm) with headspace capillary gas chromatography. The temperature was programmed. The carrier gas was nitrogen and the flow rate was 2.5 ml · min -1. Inlet temperature was 200 ° C; detector was FID detector with detector temperature of 250 ° C; headspace sampling, headspace flask equilibrium temperature was 95 ° C, equilibration time was 30 min. Using DMF as solvent, the amount of 7 residual solvents was determined by external standard method, and the injection volume was 1 ml. Results: Under these chromatographic conditions, all the seven organic solvents could be well separated. The linear relationship between the solvents and the peak area was good (r≥0.994 4) and the average recovery was 98.72% ~ 99.91% (RSD 0.14% -0.71%) (n = 9). Conclusion: The method is simple, rapid and sensitive. It can be used for simultaneous determination of organic solvent residues in Shengxuening tablet.