气相色谱内标法测定香料用鸢尾中的鸢尾酮

Quantitative analysis of irones in Iris species used for perfume production by GC with internal standard

目的:建立测定香料用鸢尾中鸢尾酮含量的气相色谱内标法。方法:样品经索式提取后,以α-紫罗兰酮为内标物,以毛细管气相色谱内标法测定样品中α-鸢尾酮与γ-鸢尾酮的含量。色谱条件:采用Rtx-1毛细管柱(30 m×0.25 mm,0.25μm),程序升温(起始温度70℃,以5℃·min-1速率升到340℃,保持5 min),载气为氮气,检测器为FID,检测器温度220℃,进样口温度200℃。结果:在选定色谱条件下,α-鸢尾酮和γ-鸢尾酮浓度分别在5.45～174.4μg·mL-1(r=0.9995)及6.10～183.0μg·mL-1(r=0.9998)范围内有良好的线性关系。平均回收率(n=6)分别为96.53%和97.16%。结论:该方法简便、灵敏、准确,可用于香料用鸢尾中鸢尾酮含量的测定。

To develop a GC method with internal standard for quantitative determination of irones in Iris species used for perfume production. Methods：The sample was extracted by Soxhlet extraction. Using a - ionone as internal standard, the contents of a - irone and γ - irone were determined with the Rtx - 1 capillary column （30 m × 0.25 mm, 0. 25 μm）. The temperature program of column was set as follows： the initial temperature was 70 ℃, then increased to 340 ℃ at a rate of 5 ℃· min - 1 and maintained for 5 minutes, and the FID flame ionization detector was used with the detector temperature at 220 ℃. The injector temperature was set at 200 ℃. Nitrogen was used as the carrier gas. Results：Under certain chromatogram condition,the calibration curves of a - irone and Y - irone were linear in the concentration ranges of 5.45 - 174.4 μg · mL-1 （r = 0. 9995 ） and 6. 10 - 183.0 μg· mL-1 （ r = 0. 9998 ）, respectively. The average recoveries （ n = 6 ） were 96.53% and 97.16%. Conclusion： The method is simple, sensitive and accurate, and can be used for quantitative determination of irones in Iris species used for perfume production.