GC测定越橘提取物中的有机溶剂残留量

Determination of Residual Organic Solvents in Bilberry Extract by GC

关键词:  越橘提取物  残留溶剂  毛细管气相色谱  顶空进样

Key words:  bilberry extract  residual solvents  GC  headspace injection

摘要:

目的 采用毛细管气相色谱法测定越橘提取物中的甲醇、乙醇、丙酮3种有机溶剂残留量。方法 采用HP-INNOWAX(30 m×0.320 mm，0.50 μm)毛细管色谱柱，氢火焰离子化检测器，程序升温：初始化温度40 ℃(维持6 min)，以25 ℃·min^-1速率升温至220 ℃(维持5 min)；载气为氮气，进样口温度：220 ℃；检测器温度：250 ℃。结果 3种有机溶剂完全分离，浓度在考察范围内与峰面积具有良好的线性关系，其中甲醇、乙醇、丙酮的线性范围分别为1.035~10.35，10.018~100.18，0.259~2.59 μg·mL^-1，平均回收率分别为97.95%，98.24%，98.10%。结论 本方法灵敏、准确、可靠，能较好地检测越橘提取物中有机溶剂残留量，控制产品质量。

Abstract:

OBJECTIVE To establish a method of headspace capillary GC for determination of residual organic solvents including methanol, ethanol and acetone in bilberry extract. METHODS The residual organic solvents were separated on HP-INNOWAX capillary column(30 m×0.320 mm, 0.50 μm). FID was used as detector with a temperature of 250 ℃, and the inlet temperature was 220 ℃. The carrier gas was nitrogen, and the flow rate was 2.0 mL·min^-1. The programmed column temperature was set as follows: maintained at 40 ℃ for 6 min and raised to 220 ℃ at the rate of 25 ℃·min^-1, followed by holding for 5 min. RESULTS the linear range of methanol, ethanol and acetone was 1.035-10.35, 10.018-100.18, 0.259-2.59 μg·mL^-1, with the average recovery of 97.95%, 98.24% and 98.10%, respectively. CONCLUSION the detection method is sensitive, accurate and reliable, and can be used in the quality control of bilberry extract.