固相微萃取三重四极杆串联质谱法检测IPA啤酒中的果香硫醇

Determination of fruit aroma thiols in IPA beer by solid-phase microextraction coupled to gas chromatography-triple quadrupole mass spectrometer

建立了三重四级杆串联质谱（GC-MSMS）结合固相微萃取技术（SPME）检测IPA啤酒、麦汁及酒花萃取液中的果香硫醇的方法。采用100μm PDMS纤维,先将纤维插入装有15 m L样品及5 g Na Cl的20 m L顶空瓶中,在室温（25℃）萃取180 min。采用GC-MSMS多反应监测扫描（MRM）模式,果香硫醇在线性范围内其响应值与浓度有较好的线性关系,相关系数达到0.993以上。样品测得值相对标准偏差（RSD%）为4.2%~6.3%（n=5）,回收率98.5%~101.4%（n=3）。实验了萃取纤维、Na Cl添加量、p H及萃取时间对果香硫醇测量值的影响。该方法可用于酒花萃取液、麦汁及啤酒的风味研究与产品质量控制及检测Cascade酒花萃取液及IPA麦汁与成品啤中果香硫醇的含量。

A new method for the determination of fruit aroma thiols in IPA beer,wort and hop by solid-phase microextraction（ SPME） coupled to gas chromatography-triple quadrupole mass spectrometry was described. The microextraction procedure was performed on PDMS fibers 100 μm. The PDMS fiber was dipped into a 20 m L vial contained 15 m L sample and 5 g Na Cl,and incubated at room temperature（ 25 ℃） for 180 min. Using GC-MS /MS on the MRM mode,the response of fruit aroma thiols exhibited good linear correlations with,and the calibration coefficients were all above 0. 993. The relative standard deviations（ RSD） and recovery for samples were 4. 2% ~ 6. 3%（ n = 5） and 98. 5% ~ 101. 4%（ n = 3）,respectively. The impact of the extraction fiber,Na Cl,p H value and extraction time on the measured values of fruit aroma thiols was also discussed. This method can be used for the determination of fruit aroma thiols in Cascade hop extracts,IPA wort and product beer,and provides a powerful tools in the flavor research and product quality control of hop,wort and product beer.