顶空气相色谱法测定反式帕罗醇中6种有机溶剂残留量

Determination of Six Residual Organic Solvents in Trans-Paroxol by Headspace Gas Chromatography

目的建立测定反式帕罗醇中6种有机溶剂残留量的方法。方法采用顶空气相色谱法,色谱柱为DB-624毛细管柱(30m×530μm,3.0μm),载气为氮气,分流比为5:1,以二甲基甲酰胺(DMF)为溶剂,程序升温,初始柱温为40℃,保持12min,然后以10℃/min的速率升温至160℃,保持3min,进样口温度为220℃,氢火焰离子化检测器(FID)温度为250℃。结果丙酮、异丙醇、石油醚、乙酸乙酯、甲苯和四氢呋喃6种有机溶剂均得到有效分离,回收率及线性关系皆良好。结论该方法灵敏度、准确性均达到有机溶剂残留量的检测要求,可用于测定反式帕罗醇中有机溶剂的残留量。

Objective To establish a method for determining the residual organic solvents in trans-paroxol. Methods The quantification by the headspace gas chromatography was as follows： using DB-624 capillary column（30 m × 530μm, 3.0μm）, nitrogen as carrier gas, the analysis was carried out at the split rate of 5 ： l,dimethylformamide （DMF） was used as the solvent,the oven temperature was beginning from 40 ℃ ,after maintaining 12 min,the temperature was programmatically increased to 160℃ at the rate of 10℃ min and maintained for 3 min. The injection port temperature was 220℃ and the detector temperature was 250℃. Results The six residual organic solvents consisting of acetone, isopropanol, petroleumether, ethyl acetate, toluene and tetrahydrofuran were completely separated, the recovery rate and linear relationship were good. Conclusion The proposed method meets the detecting demand in accuracy and sensitivity for residual organic solvents,wilich indicates it is suitable to the determination of residual organic solvents in transparoxol.