顶空气相色谱法检测石茶感冒胶囊中的有机溶剂残留

Determination of residual organic solvents in Shicha Ganmao Capsule by gas chromatography with headspace sampling

目的建立石茶感冒胶囊中可能残留的7种有机溶剂(正己烷、苯、甲苯、对二甲苯、邻二甲苯、苯乙烯、二乙烯苯)的检测方法。方法采用顶空气相色谱法,色谱柱为AgilentHP-INNOWAX毛细管柱(30m×1.0mm,0.53μm),载气为高纯氮气;顶空温度为70℃,顶空时间30min;柱温自30℃恒定5min,以10℃/min升温速率升至200℃,恒定5min;氢火焰离子检测器(FID),温度为250℃。结果7种有机溶剂残留物在所考察的浓度范围内线性关系良好(r=0.9994～0.9998),精密度RSD均小于5.0%,被测组分的平均回收率在99.16%～102.0%之间。结论该方法操作简便、快速、准确度高,可用于检测石茶感冒胶囊中的有机溶剂残留物。

Objective To establish a method for determination of the seven residual organic solvents （nhexane, benzene, toluene, o-dimethylbenzene, p-dimethylbenzene, styrene and divinyl benzene） in Shicha Ganmao Capsule. Methods Gas chromatography with headspace sampling was applied to the study. Agilent HP-INNOWAX silica capillary column was 30 m × 1.0 mm, 0.53 μm. The initial temperature was kept at 30 ℃ for 5 min, then the temperature was raised to 200 ℃ at the rate of 10 ℃/min and subsequently sustained for 5 min. FID detector temperature was 250 ℃. The vial temperature was 70 ℃, and the vial time was 30 min. Results There was a good linearity in the experimental concentration （r= 0. 999 4- 0. 999 8）. The RSD was all less than 5.0%. The average recovery rates were in the range of 99.16%- 102.0%. Conclusion The analytical method is simple, accurate and sensitive.