黔产毛蒟挥发油的提取工艺优化及化学成分分析

摘要

OBJECTIVE:To optimize the extraction technology of volatile oil from Guizhou Piper puberulum and analyze its chemical compositions. METHODS:The volatile oil was extracted from Guizhou P. puberulum by steam distillation(HD method). Orthogonal test was designed using the extract rate of volatile oil as index,with soaking time,extraction time,material-liquid ratio (g/ml) and smashed particle size as factors. Validation test was also conducted. GC-MS was adopted to separate and identify the chemical compositions of the volatile oil from Guizhou P. puberulum,and area normalization method was used for the determina-tion of relative percentage of each composition. RESULTS:The optimal extraction technology was as follows as soaking time of 3 h,extraction time of 5 h,material-liquid ratio of 1∶10 and degree of grinding 12 meshes;in validation test,average extract rate of volatile oil was 59.83%(RSD=0.905 3%,n=3). 78 compounds were identified,and relative percentage was 81.125%;there were four main compositions such as γ-elemene(11.858%),4-vinyl-α,4-trimethyl-3-(1-methylvinyl)-cyclohexane methanol(8.701%), carnation(8.443%)and α-caryophyllene(6.216%). CONCLUSIONS:Optimized HD method is simple in production equipment, low in production cost,good in repeatability;determination method of validation oil is simple and feasible,and can analyze chemi-cal compositions of volatile oil from Guizhou P. puberulum.%目的：优化黔产毛蒟挥发油的提取工艺并分析其化学成分。方法：采用水蒸气蒸馏法（HD）提取黔产毛蒟挥发油。以挥发油提取率为考察指标，以浸泡时间、提取时间、料液比（g/ml）、粉碎程度为考察因素设计正交试验；同时进行验证试验。采用气相色谱-质谱联用法对黔产毛蒟挥发油的化学成分进行分离鉴定，并以面积归一化法测定各成分的相对百分含量。结果：最优提取工艺为浸泡时间3 h、提取时间5 h、料液比1∶10、粉碎程度12目；验证试验中挥发油平均提取率为59.83％（RSD＝0.9053％，n＝3）。共鉴定出78种化合物，相对百分含量为81.125％；其中γ-榄香烯（11.858％）、4-乙烯基-α，4-三甲基-3蒟（1-甲基乙烯基）-环己烷甲醇（8.701％）、石竹（8.443％）、α-石竹烯（6.216％）等4种化合物为主要成分。结论：优化的HD法生产设备简单、生产成本低廉、重现性好；挥发油成分分析方法简单、可行，可对黔产毛蒟挥发油的化学成分进行分析。