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目的建立以顶空气相色谱法测定聚普瑞锌原料药中甲醇、乙醇、三氯甲烷和甲苯4种有机溶剂残留量的方法。方法以1 mol·L~(-1)硫酸溶液为溶剂,采用Agilent DB-FFAP(30 m×0.32 mm,0.5μm)毛细管柱,载气为氮气,柱流速为2 m L·min~(-1);柱温为程序升温,氢火焰离子化检测器(FID),检测器温度为250℃;进样口温度为200℃;顶空瓶平衡温度为80℃。结果甲醇、乙醇、三氯甲烷和甲苯均能较好的分离,呈现良好的线性关系,平均回收率分别为102.9%,105.4%,93.8%,95.7%,RSD分别为2.9%,2.1%,3.3%,3.5%(n=9)。结论本方法简便快速,准确性好,灵敏度高,可用于聚普瑞锌原料药中残留溶剂的测定,同时也为难溶性原料药中的残留溶剂测定提供一个思路。
OBJECTIVE To establish a method for the determination of residual organic solvents in methanol, ethanol, trichloromethane and toluene by HPLC using headspace gas chromatography. Methods A capillary column with Agilent DB-FFAP (30 m × 0.32 mm, 0.5 μm) was used as the solvent in 1 mol·L -1 sulfuric acid solution. The carrier gas was nitrogen and the column flow rate was 2 m L · min ~ (- 1); column temperature programmed temperature, flame ionization detector (FID), detector temperature of 250 ℃; inlet temperature of 200 ℃; headspace bottle equilibrium temperature of 80 ℃. The results showed that methanol, ethanol, chloroform and toluene could all be separated well and the average recoveries were 102.9%, 105.4%, 93.8% and 95.7%, respectively. The RSDs were 2.9%, 2.1%, 3.3% %, 3.5% (n = 9). Conclusion The method is simple and rapid, accurate and sensitive. It can be used for the determination of residual solvents in the preprimary zinc drug substance, and provides a new idea for the determination of residual solvents in the insoluble drug substance.