GC-MS分析不同产地香荚兰商品荚乙醇提取物化学成分差异及其香草醛的测定

Analysis on chemical constituents in ethanol extract from vanilla pod in various habitats and quantitative determination of vanillin by GC-MS

目的分析中国海南与巴布亚新几内亚所产香荚兰商品荚乙醇提取物中化学成分的差异并测定香草醛的量。方法对不同样品处理方法进行比较,采用GC-MS分析法,利用Agilent DB-5MS弹性石英毛细管柱(30 m×0.32 mm,0.25μm),在初始温度为60℃,保持1 min,以10℃/min升至260℃,保持6 min,再以6℃/min升至290℃,保持8 min;载气为氦气的条件下,对比两产地乙醇提取物的差异。结果两产地所产香荚兰商品荚乙醇提取物中分别鉴定出34和32种化合物,其中共有化合物18种。香草醛在香荚兰商品荚中的相对质量分数较高,定量测定结果表明,在质量浓度0.04～1.10 mg/mL内与峰面积呈良好的线性关系(r=0.999 8,n=5);回收率为100.05%,RSD为1.88%。结论本方法能快速、简便、高效地检测出香荚兰商品荚乙醇提取物的化学成分,并且在香草醛的定量测定中具有稳定、可重复的特点。

Objective To analyze the chemical constituents in ethanol extracts from vanilla pod in Hainan （China） and Papua-New Guinea and to assay the content of vanillin. Methods Comparing various pretreatment methods, GC-MS analysis method was selected and the column was packed with Agilent DB-5MS capillary column （30 m × 0.32 mm, 0.25 gm）; column temperature： the column initial temperature was 60 ℃, kept for 1 min, rose to 260 ℃ at the rate of 10 ℃/min, kept for 6 min, rose to 290 ℃ at the rate of 6℃/min, kept for 8 min; carrier gas： helium for comparing the difference of the constituents from the aboVe two habitats. Results Because of the different habitats, 34 and 32 compounds were respectively identified from vanilla pod and 18 compounds were common components. Vanillin had a high content in vanilla pod and presented a good linearity with the peak area at the concentration of 0.04-- 1.10 mg/mL （r = 0.999 8, n = 5）. The average recovery was 100.05% with the RSD of 1.88%. Conclusion GC-MS is quick, simple, convenient, and effective to analyze the constituents in the ethanol extracts from vanilla pod, and it is also reliable and reproducible to determine the content of vanillin.