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基于SPE-GC-MS技术同时测定酱香型白酒中13种萜烯类化合物OA

Simultaneous determination of 13 terpenes in sauce-flavor Baijiu based on SPE-GC-MS technology

中文摘要英文摘要

该研究建立了采用固相萃取(SPE)结合气相色谱-质谱(GC-MS)同时检测酱香型白酒中13种萜烯类化合物含量的方法.样品经C18固相萃取小柱及Florisil固相萃取小柱串联上样、分别洗脱的方式净化浓缩,DB-5毛细管色谱柱(30m×0.25 mm×0.25 μm)分离,选择离子监测(SIM)模式结合内标法定量,并采用该方法检测贵州不同工艺酱香型白酒中各萜烯类化合物含量的差异.结果表明,13种萜烯类化合物在各自质量浓度范围内线性关系良好,相关系数(R2)≥0.994,检出限(LOD)为0.05~7.14 μg/L,定量限(LOQ)为0.16~23.81 μg/L,平均加标回收率为81.0%~104.8%,精密度试验结果的相对标准偏差(RSD)为4.28%~9.26%.不同工艺酒样中萜烯类化合物的总含量存在差异,但芳樟醇、香叶基丙酮含量较高,含量分别为1.52~3.10 mg/L和0.71~3.50 mg/L.该方法前处理操作简单、灵敏度高,准确性和精密度良好,可同时测定酱香型白酒中13种萜烯类化合物.

A method for the simultaneous determination of the contents of 13 terpenes in sauce-flavor(Jiangxiangxing)Baijiu was established by solid-phase extraction(SPE)combined with gas chromatography-mass spectrometry(GC-MS).The samples were purified and concentrated by C18 and Florisil solid-phase extraction cartridges in tandem,separated by DB-5 capillary chromatography column(30 m×0.25 mm×0.25 μm),and quantified by selected ion monitoring(SIM)mode combined with the internal standard method.The results showed that all 13 terpenes exhibited a good linear relationship within their respective mass concentration ranges,with the correlation coefficient(R2)≥ 0.994.The limits of detection(LOD)were 0.05-7.14 μg/L,and the limits of quantification(LOQ)were 0.16-23.81 μg/L,the average spiked recovery rates were 81.0%-104.8%,and the relative stan-dard deviations(RSD)of the precision test results were 4.28%-9.26%.The total content of terpene compounds in Baijiu samples with different pro-cesses was different,but the contents of linalool and geraniol were relatively high,which were 1.52-3.10 mg/L and 0.71-3.50 mg/L,respectively.This method featured simple pretreatment operations,high sensitivity,good accuracy and precision,and could be used for the simultaneous determination of 13 terpenes in sauce-flavor Baijiu.

黄家岭;张吉敏;杨金川;张倩;孙棣;李春宇;廖妍俨;周心;阮晓

贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001贵州省产品质量检验检测院,贵州 贵阳 550001

轻工纺织

萜烯类化合物固相萃取气相色谱-质谱酱香型白酒

terpenessolid-phase extractiongas chromatography-mass spectrometrysauce-flavor Baijiu

《中国酿造》 2026 (2)

293-300,8

贵州省产品质量检验检测院科研项目[院科(2022)006号]

10.11882/j.issn.0254-5071.2026.02.041

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