三种萃取方法对模拟葡萄酒中单萜类化合物GC-MS分析的影响

Effects of three extraction methods on GC-MS analysis of monoterpenoids on simulated wines

【目的】筛选出检测单萜类化合物的较佳方法,并对相关参数进行优化,以期提高单萜类化合物的检测效率和准确性,为葡萄酒中单萜类化合物的分析鉴定提供技术支持.【方法】采用液-液萃取(LLE)、固相萃取(SPE)和顶空-固相微萃取(HS-SPME)3种不同的萃取方法,结合气相色谱-质谱联用仪(GC-MS)分析模拟葡萄酒中的4种单萜类化合物(芳樟醇、香茅醇、橙花醇、香叶醇),对不同萃取方法的重复性、检测限和回收率进行比较.【结果】与其他两种方法相比,HS-SPME法最佳,平均RSD值为1.65%,检测限为0.12~0.62μg/L,回收率92.6%~102.3%.优化的HP-SPME法萃取条件为:20mL进样小瓶中加入10mL酒样,选用DVB/CAR/PDMS纤维萃取头,60℃恒温水浴萃取30min后进GC-MS分析.用HS-SPME方法定量分析了‘贵人香’干白葡萄酒中的目标化合物,平均加标回收率(97.43%~101.66%)和精密度(4.80%~7.50%)良好.【结论】采用HS-SPME法结合GCMS更适合于葡萄酒中单萜类化合物的检测.

[Objective] To screen out the better method to determine the monoterpenes in wine and to promote the detection efficiency and veracity. [Method] Three different extraction methods were carried out by liquid liquid extration （LLE）, solid phase extraction （SPE） and headspace solid phase microextraction （HP SPME）. Four monoterpenes in the simulated wine （linalool, citronellol, nerol, geraniol） were analyzed by gas chromatography mass spectrometry （GC-MS）. The reproducibility and detection limit and recovery rate of different extraction methods were compared. [Resultl The method of HS SPME showed the best, the average RSD was 1.65 %, the detection limit was O.12 ~ 0.62 μg/L, and the recovery rate was between 92. 6 % and 102. 3 %. The optimum conditions of HS SPME were 20 mL of the sample was added to the 20 mL sample vial. The extraction fiber was DVB/CAR/PDMS. The fiber was sealed for 30 min at 60 ℃ in water bath. The method was used to determine the monoterpenes content in dried white wine. The average recovery rate was 97.43 % ~ 101.66 % and the precision was 4.80 % ~ 7.50 %. [Conclusion]HS-SPME combined with GC MS show better performance for the detection of monoterpenoids in white wine.