气相色谱法测定葡萄内酯中的溶剂残留

Determination of residual solvents in auraptene by gas chromatography

目的：建立葡萄内酯中3种有机溶剂残留测定方法。方法：采用毛细管气相色谱法，FID检测器，应用DM．WAX毛细管柱（30m×0．25mm×0．25μm），载气为氮气，柱温采取程序升温，初始温度40℃，保持4min，然后以40／min升至200℃，保持1min，测定葡萄内酯中丙酮、甲醇和吡啶的残留量。结果：被测组分均能得到有效分离，在所考察的浓度范围内线性关系良好，r=0．9995—0．9999，平均回收率为96．25％～99．58％。结论：本方法灵敏、准确、可靠，可用于葡萄内酯中有机溶剂的检测。

Objective：To establish a method for determination of three residual solvents in auraptene. Methods：The determination was performed on DM-WAX（ 30m × 0.25 mm × 0.25 μm ） capillary. Samples were separated with capillary column programmed increased temperature and analyzed with FID detector at 250 ℃. The initial temperature was kept at 40 ℃ for 4 min, then the temperature was raised to 200 ℃ at the rate of 40 ℃/min and kept for 1 min. Result ： There was a good linearity （ r = 0. 9995 - 0.9999） and three residual solvents were completely separated. The average recovery rate was in the range of 96.25 -99.58%. Conclusion：The method is aeeurate and sensitive and can be used for determination of three residual solvents in auraptene.