LLE-GC-MS-SIM检测白酒中9 种微量功能成分

应用液液萃取（liquid-liquid extraction，LLE）结合气相色谱-质谱-选择离子扫描（gas chromatography-mass spectrometry-selective ion monitoring，GC-MS-SIM）技术检测20 种白酒中D-柠檬烯、对伞花烃、叶绿醇、4-甲基愈创木酚、4-乙基愈创木酚、麝香草酚、异丁香酚、四甲基吡嗪及亚油酸乙酯含量。该方法回收率在81.80%～109.30%之间，精密度均小于6.00%；检测范围内，线性关系良好（R2＞0.999 0），检出限和定量限分别为0.17～0.91 μg/L和0.58～3.04 μg/L。LLE-GC-MS-SIM法对9 种功能成分的定量检测结果表明，3 种萜烯类物质在浓香型酒样中含量较高，且山庄酒厂酒样含量普遍高于市售酒样；芝麻香型白酒中酚类物质含量最高，其中酒样W09中4 种酚类物质质量浓度高达4 301.61 μg/L；四甲基吡嗪在酱香型酒样中质量浓度为2 379.65～2 985.09 μg/L，远高于芝麻香型酒样的1 116.80～1 309.66 μg/L及浓香型酒样的245.40～555.76 μg/L；亚油酸乙酯在不同酒样中含量差异较大，除市售酒样W17、W19和W20外，其余酒样质量浓度为1 951.96～7 183.35 μg/L。

Determination of Nine Trace Functional Components in Chinese Baijiu by Liquid-liquid Extraction Coupled to Gas Chromatography-Mass Spectrometry-Selective Ion Monitoring

Totally nine volatile trace components in 20 samples of different kinds of Chinese Baijiu were analyzed by liquid-liquid extraction (LLE) combined with gas chromatography-mass spectrometry-selective ion monitoring (GC-MS-SIM). The average recoveries of the developed method were in the range of 81.80%–109.30%, with a precision (relative standard deviation, RSD) of less than 6.00%. Excellent linearity was observed in the tested concentration range (R2 > 0.999 0). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.17–0.91 and 0.58–3.04 μg/L, respectively. The results showed that among the nine functional compounds, three terpenes had higher concentrations in Nongxiangxing Baijiu, and their concentrations in the Baijiu samples from a producer in Chengde, Hebei were higher than those in other samples examined. Four phenolic compounds had the highest concentrations in Zhima-flavor Baijiu, and the total amount of phenolics was 4 301.61 μg/L in sample W09. The concentration of tetramethylpyrazine in Jiang-flavor Baijiu was 2 379.65–2 985.09 μg/L, much higher than that in Zhima-flavor Baijiu (1 116.80–1 309.66 μg/L) and Nongxiangxing Baijiu (245.40–555.76 μg/L). The concentration of linoleic acid ethyl ester significantly varied in the range of 1 951.96–7 183.35 μg/L among different samples expect for W17, W19 and W20.