SPME-GC-MS测定‘凤丹’牡丹籽油挥发物组成时固相微萃取条件的响应面优化Response surface optimization of solid phase microextraction condition for the determination of volatiles in Fengdan seed oil by SPME-GC-MS

为‘凤丹’牡丹籽油风味研究提供参考，采用固相微萃取技术结合气相色谱-质谱法（SPME-GC-MS）测定‘凤丹’牡丹籽油挥发物组成。在单因素试验基础上，根据Box-Behnken试验设计原理，以‘凤丹’牡丹籽油挥发物总峰面积为响应值，以样品量、平衡时间、萃取时间、萃取温度为因素进行响应面试验，对‘凤丹’牡丹籽油挥发物的固相微萃取条件进行优化，然后采用SPME-GC-MS测定‘凤丹’牡丹籽油的挥发物组成及相对含量。结果表明：固相微萃取‘凤丹’牡丹籽油挥发物的最佳条件为样品量4.0 g（15 mL样品瓶），平衡时间40 min，萃取时间20 min，萃取温度80 ℃；在最佳条件下结合GC-MS分析测得‘凤丹’牡丹籽油中共有22种挥发物，其中烯烃类、酯类、醛类、醇类、杂环类、芳烃类和酚类的相对含量分别为33.34%、21.12%、20.76%、19.05%、3.48%、1.67%、0.61%。综上，该响应面法优化的固相微萃取条件适合快速测定‘凤丹’牡丹籽油挥发物，烯烃类、酯类、醛类和醇类是‘凤丹’牡丹籽油中的重要挥发物。 In oder to provide reference for the study of flavor of Fengdan seed oil, the volatile composition of Fengdan seed oil was determined by solid-phase microextraction combined with gas chromatography-mass spectrometry (SPME-GC-MS). On the basis of the single factor experiment, according to the Box-Behnken experimental design principle, with the total peak area of volatile in Fengdan seed oil as the response value, the response surface methodology was conducted to optimize the conditions for the solid-phase microextraction of volatiles in Fengdan seed oil, with the sample amount, equilibrium time, extraction time, and extraction temperature as the factors. Then the volatile composition and relative content of Fengdan seed oil were determined by SPME-GC-MS. The results showed that the optimal conditions for solid phase microextraction of the volatiles in Fengdan seed oil were obtained as follows: sample amount 4.0 g(15 mL sample flask), equilibrium time 40 min, extraction time 20 min, and extraction temperature 80 ℃. Under the optimal conditions and combined with GC-MS analysis, 22 kinds of volatiles in Fengdan seed oil were detected. Among them, the relative contents of alkenes, esters, aldehydes, alcohols, heterocyclics, aromatic hydrocarbon and phenols were 33.34%, 21.12%, 20.76%, 19.05%, 3.48%, 1.67% and 0.61%, respectively. In conclusion, the solid phase microextraction conditions optimized by the response surface methodology are suitable for rapid determination of volatile in Fengdan seed oil, and alkenes, esters, aldehydes and alcohols are important volatile compounds in Fengdan seed oil