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目的:采用简单快速的顶空单滴微萃取-气相色谱法分析测定百草油中挥发性成分薄荷醇和水杨酸甲酯含量。方法:精密吸取样品的甲醇溶液10μL注入盛有5 mL水的样品瓶中,以1.5μLN,N-二甲基甲酰胺为萃取溶液(含内标苯甲醇),萃取温度为40℃、萃取时间为5 min,萃取后直接吸回0.5μL进样GC分析检测。采用30 m×0.53 mm PEG毛细管柱,FID检测器,程序升温。结果:薄荷醇、水杨酸甲酯和其他成分的分离度良好,加样回收率在95.4%~99.2%,RSD均低于1.9%。薄荷醇和水杨酸甲酯分别在1.26~80.5(r=0.999 0),2.49~1.59×102mg.L-1(r=0.999 1)线性关系良好。结论:该方法避免了复杂的样品前处理,操作简单快速,定量准确,且成本低,适用于中药中挥发性成分的含量测定。
OBJECTIVE: To determine the content of menthol and methyl salicylate in the essential oil of Paeonia by using simple and rapid headspace single drop microextraction-gas chromatography. Methods: 10 μL of methanol solution of precision aspirate sample was injected into a vial containing 5 mL of water, 1.5 μL of N, N-dimethylformamide as extraction solution (containing internal standard benzyl alcohol), extraction temperature of 40 ℃, extraction time For 5 min, directly extracted after extraction 0.5μL injection GC analysis and detection. Using 30 m × 0.53 mm PEG capillary column, FID detector, the program temperature. Results: The separation of menthol, methyl salicylate and other components was good with recoveries of 95.4% -99.2% and RSDs less than 1.9%. There was a good linear relationship between menthol and methyl salicylate in the range of 1.26-80.5 (r = 0.999 0) and 2.49-1.59 × 102 mg.L-1 (r = 0.999 1). Conclusion: This method avoids complicated sample preparation, simple and fast operation, accurate quantification, low cost and suitable for the determination of volatile components in traditional Chinese medicine.