通过对顶空固相微萃取(headspace-solid phase microextraction,HS-SPME)、同时蒸馏萃取(simultaneous distillation-extraction,SDE)和液液萃取(liquid-liquid extraction, LLE)3种提取方式的选择、优化,建立了液液萃取结合气相色谱-质谱对山药酒中萜烯类化合物的分析方法。经方法学评估,各萜类化合物线性良好(R2≥0.993 6),定量限为1.86~89.88 μg/L,相对标准偏差小于1.7%,加标回收率为92.68%~103.21%。采用该方法对市售3类山药酒进行分析,准确定量了10种萜烯类化合物,包括5种单萜类化合物、3种倍半萜类化合物以及二萜类化合物和三萜类化合物各1种;各类山药酒中萜烯类化合物组成相近,含量存在差异,与原料产地和加工工艺具有一定的相关性,含量较丰富的长叶松烯、(-)-龙脑、香茅醇和角鲨烯等赋予了山药酒独特的风味及保健功效,为深入研究山药酒的活性成分提供数据支撑。
By selecting and optimizing three extraction methods: headspace-solid phase microextraction (HS-SPME), simultaneous distillation-extraction (SDE), and liquid-liquid extraction (LLE), LLE coupled with GC-MS was developed and applied to determine terpenoids in yam wine. The established methodology displayed a good linear relationship (R2≥0.993 6) of each terpenoid. The quantification limit of the method was in a range of 1.86-89.88 μg/L, the RSD value was less than 1.7%, and the recovery rate was in a range of 92.68%-103.21%. A total of ten terpenoids were accurately quantified by this method in three types of commercial yam wine, including five monoterpenoids, three sesquiterpenes, one diterpenoids, and one triterpenoids. The composition of terpenoids in each yam wine was similar, but their contents were different, which had certain correlations with the origin of raw materials and the processing technology. The major components were longifolene, (-)-borneol, citronellol, and squalene, which provide yam wine unique flavor and health functions. This study provides data support for further studying the active ingredients of yam wine.
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