盐析辅助水蒸气蒸馏法制备红松壳挥发油研究

采用盐析辅助水蒸气蒸馏法(salt out-assisted steam distillation,SOSD)制备红松壳挥发油,探讨无机盐对蒸馏方式的影响,通过单因素试验研究了蒸馏时间、固液比、无机盐、磷酸氢二钠的质量浓度、萃取剂等因素对红松壳挥发油提取率的影响,并采用气相色谱-质谱联用技术对红松壳挥发油成分进行分析。结果表明:SOSD法最佳制备工艺条件为蒸馏时间3 h,固液比1:9(g/mL),盐析效果最好的无机盐为4×10-3 g/mL磷酸氢二钠,在此条件下红松壳挥发油提取率为0.9%,是水蒸气蒸馏法(steam distillation,SD)制备红松壳挥发油提取率(0.64%)的1.4倍。红松壳挥发油成分分析表明:SOSD法提取红松壳挥发油共分析出17种可能成分,而SD提取红松壳挥发油共分析出16种可能成分,两种方法提取结果有9种相同可能成分,如反-α反-α,α-5-三甲基-5-乙烯基四氢化-2-呋喃甲醇、苯甲醛、左旋樟脑、2-茨醇、(1R)-(+)-诺蒎酮、2,6,6-三甲基双环[3.1.1]庚-2-烯、2-(4-甲基苯基)丙-2-醇、4,6,6-三甲基二环[3.1.1]庚-3-烯-2-酮、3-甲基-6-(1-甲基亚乙基)-2-环己烯-1-酮等,其相对百分含量差别不大。
The volatile oil of pine shell was extracted by salt out-assisted steam distillation to discuss effect of inorganic salt in the process of steam distillation. The distillation time, solid-liquid ratio, the inorganic salt type and its concentration, extraction agent on the yield of pine shell volatile oil were studied by single factor tests, while the constituents of pine shell volatile oil was analyzed by the gas chromatograph/mass spectrom(GC/MS). The results showed that the optimized extraction technology of the salting out-assisted steam distillation was distillation time for 3 h, solid-liquid ratio for 1:9(g/mL), best salting out effect was 4×10-3 g/mL disodium hydrogen phosphate. The yield of volatile oil was up to 0.9% under these conditions, that is steam distillation method prepared pine shell volatile oil extraction rate(0.64%)of 1.4 times. The results of pine shell volatile oil components analysis showed that 17 species components in the pine shell volatile oil prepared by salting out-assisted steam distillation were identified by GC/MS, and 16 species components in the pine shell volatile oil prepared by steam distillation. There are the same nine species components in two kinds of essential oil, 2-furanmethanol,5-ethenyltetrahydro-5-trimethyl; benzaldehyde; bicyclo[2.2.1]heptan-2-one, 1,7,7-trimethyl-,(1S); bicyclo[2.2.1]heptan-2-ol,1,7,7-trimethyl; bicyclo[3.1.1]heptan-2-one,6,6-dimethyl-,(1R); bicyclo[3.1.1]heptan-2-one,3,6,6-trimethyl, benzenemethanol,4-trimethyl; bicyclo[3.1.1]hept-3-en-2-one,4,6,6- trimethyl, 2-cyclohexen-1-one,3-methyl-6-(1-methylethenyl). The relative percentage of 9 kinds of components is almost equal