采用HS-SPME-GC-MS法对玫瑰饮品香气成分的定量研究

摘要

Headspace solid phase microextraction (HS-SPME) combined with gas chromatography- mass spec- trometry has been applied for analysing 19 aroma compounds in rose beverage to optimize rose brewing technology. These compounds contained aromatics, terpenoids, terpenoid derivative, and alkanes. The optimization of HS-SPME combined with standard addition quantification was carried out. The correlation coefficients were from 0. 9901 to 0. 9995. The precision and recovery ranged from 0.88% to 15.21% and from 83.93% to 112.02% , respectively. The detection limit was from 0.02 to 13.32μg/L. It demonstrated that the method was a promising technique. 5 rose bev- erages were determined. The results showed that the concentration of compounds were different in different samples. 2-phenylethanol was the most abundant component. It accounted for 78.55% ~ 96.03% with the concentration from 64318.00μg/L to 195203. 47μg/L. The other major compounds were citronellol, methyl eugenol, eugenol, and gera- niol, accounting for 0.21% - 6.14% with the concentration from 170.0μg/L to 7005.90μg/L. The minor com- pounds were citronellyl acetate, nerol, rose oxide and nerolidol with the concentration from dozens of μg/L to 300~g/ L. In addition, some terpenoids and alkanes were low with dozens of I.Lg/L or even lower than 1 μg/L because of their low water solubility. Statistical analysis indicated no significant difference among five rose beverage (P 〉 0.05 ). Fur- thermore, the most similar beverages were No. 2, 3, and 5. Key words rose, headspace solid phase microextraction, gas chromatography-mass spectrometry, volatile com- pounds, terpenoids, alkanes%为优化玫瑰饮品酿制工艺，采用顶空固相微萃取．气相色谱质谱联用仪分析了其中19种主要芳香成分，包括芳香族、萜类及其衍生物和烷烃类物质。通过优化各种参数，并结合标准加入法定量，该方法的相关系数为0．9901～0．9995，精密度为0．88％-15．21％，检出限为0．02～13．32μg／L，回收率为83．93％-112．02％，表明该法准确可靠。利用该法检测了5种不同种类的玫瑰饮品，发现各成分的含量虽不同，但每种化合物都是在一定范围内变化。p一苯乙醇是最主要的成分（占78．55％-96．03％），含量为64318．00～195203．47μg／L；其次是香茅醇、甲基丁香酚、丁子香酚和香叶醇，其各自比例都在0．21％～6．14％，含量为170．01～7005．90μg／L；再次是乙酸香茅酯、橙花醇、玫瑰醚和橙花叔醇，其含量为数十至300μg／L；其他化合物如部分萜类、烷烃类物质，由于它们的难溶性导致其含量很低，在数十个μg／L甚至1μg／L以下。经统计分析发现，5种玫瑰饮品中化合物含量无显著性差异，但通过聚类分析发现饮料2、3、5总体上最为相似。