琥珀油的提取及成分分析

Extraction and Component Analysis of Amber Oil

分别采用水蒸气蒸馏法和有机溶剂提取法提取琥珀挥发油(琥珀油)。在琥珀油提取过程中,考察了不同类型提取溶剂、琥珀粉碎程度、浸泡时间及提取时间等因素对琥珀油得率的影响,以及优化琥珀挥发油的提取工艺。结果表明,水蒸气蒸馏法与有机溶剂提取法相比,水蒸气蒸馏法提取琥珀油量少,纯度较高;有机溶剂提取法提取的琥珀油量多,但纯度较低。当琥珀粉粒径为1.5×10^(5)nm、提取温度为120℃,提取时间为12~14 h时,采用水蒸气蒸馏法提取出的琥珀油最为纯净,琥珀油最大得率为0.75%。通过红外光谱分析,发现琥珀油中主要含有烷烃类、脂肪酮类或饱和脂肪酸酯、芳烃类、醇和烯烃类化合物等,通过气相色谱-质谱(GC-MS)对琥珀挥发油的化学成分进行了鉴定,通过面积归一化法确定各成分的质量分数,鉴定出琥珀油中主要成分有斯巴醇(质量分数为36.74%)、α-咕巴烯(质量分数为23.84%)、氧化石竹烯(质量分数为5.25%)、马兜铃烯环氧化物(质量分数为5.02%)、β-榄香烯(质量分数为3.63%)、1,6-二烯-3-律草醇(质量分数为3.29%)、异长叶烯(质量分数为3.10%)和α-比萨波醇(质量分数为2.79%)等,琥珀挥发油各项指标符合国家标准,重金属含量较少,菌落数达标。

Amber volatile oil(amber oil)was extracted by steam distillation and organic solvent extraction,respectively.During the extraction of amber oil,the process was optimized by comparing the effects of different types of extraction solvents,amber crushing degree,soaking time and extraction time on the yield of amber oil.The results showed that the amount of amber oil extracted by steam distillation was less and the purity was higher than that by organic solvent extraction;the amount of amber oil extracted by organic solvent extraction was large,but the purity was low and contained a certain amount of impurities.When amber oil was extracted by steam distillation,the particle size of amber powder was 1.5×105 nm,the extraction temperature was 120℃and the extraction time was 12~14 h,the extracted oil was the purest,and the maximum yield was 0.75%.Through infrared spectrum analysis,it was found that amber oil mainly contains alkanes,fatty ketones or saturated fatty acid esters,aromatics,alcohols and olefins.The chemical components of amber volatile oil were identified by gas chromatography-mass spectrometry(GC-MS),and the mass fraction of each component was determined by area normalization method.The results showed that the main components in amber oil were spathulenol(mass fraction 36.74%),α-copaene(mass fraction 23.84%),caryophyllene oxide(mass fraction 5.25%),aristolochicene epoxide(mass fraction 5.02%)β-elemene(mass fraction 3.63%),1,6-diene-3-propanol(mass fraction 3.29%),iso-longifolene(mass fraction 3.10%)andα-pisapol(mass fraction 2.79%),etc.Referring to the national standard method,the density,acidity,heavy metal content and colony number of amber volatile oil were determined.The results showed that all indexes of amber volatile oil meet the national standard,the content of heavy metals is less,and the colony number reaches the standard.