摘要
采用蒸馏法结合顶空固相微萃取-气质联用(HS-SPME-GC-MS)技术测定酒醅中土味素,优化蒸馏、固相微萃取及色谱柱条件参数,以2-异丁基-3-甲氧基吡嗪为内标,建立了酱香型白酒酒醅中土味素定量检测方法。结果表明,蒸馏最佳条件为料液比1∶15;最佳色谱柱为HP-5MS;最佳进样方式为HS-SPME;HS-SPME检测最佳条件为:萃取温度60℃,萃取时间50 min,氯化钠添加量2.5 g。该方法测定酒醅中土味素在质量浓度8~160μg/L范围线性良好(R2=0.998),检出限0.0016μg/L(S/N=3),定量限0.005μg/L(S/N=10),加标回收率89.59%~105.53%。该方法准确性高、重复性好,可以广泛推广应用于酱香型白酒酒醅中土味素含量测定。
The distillation method combined with headspace solid-phase microextraction and gas chromatography-mass spectrometry(HS-SPME-GC-MS)was adopted to determine the content of geosmin in the fermented grains of Jiangxiang Baijiu.With 2-isobutyl-3-methoxypyrazine as the internal standard,the distillation parameters,HS-SPME conditions and GC-MS conditions were optimized.The results showed that the optimal material-liquid ratio for distillation was 1∶15.The optimal chromatographic column was HP-5MS.The optimal injection method was HS-SPME.The optimal HS-SPME conditions were as follows:extraction temperature of 60℃,extraction time of 50 min,and NaCl addition of 2.5 g.The method exhibited good linearity in the range of 8μg/L to 160μg/L(R2=0.998).The detection limit was 0.0016μg/L(S/N=3),the quantification limit was 0.005μg/L(S/N=10),and the recovery rate was between 89.59%and 105.53%.The method is accurate and reproducible,and can be widely used in the determination of geos-min in fermented grains.
作者
张娅
李细芬
马明娟
彭禹熙
樊双喜
尹学忠
杨礼红
侯玉祥
卢君
李长文
ZHANG Ya;LI Xifen;MA Mingjuan;PENG Yuxi;FAN Shuangxi;YIN Xuezhong;YANG Lihong;HOU Yuxiang;LU Jun;LI Changwen(Guizhou Guotai Distillery Co.Ltd.,Renhuai,Guizhou 564501;Guotai Research Academy,Tianjin 300410,China)
出处
《酿酒科技》
2024年第5期30-36,共7页
Liquor-Making Science & Technology
基金
贵州省科技成果应用及产业化计划项目(黔科合成果[2020]2Y045)
遵义市科技计划项目(遵市科合R&D[2020]31号)
遵义市科技计划项目(遵市科合支撑GY(2021)40号)
贵州省科技计划项目(黔科合成果[2023]-般149)。
关键词
顶空固相微萃取
气相色谱质谱联用法
酒醅
蒸馏
土味素
定量检测
headspace solid-phase microextraction
gas chromatography-mass spectrometry
fermented grains
distillation
geosmin
quantitative detection
