分散液液微萃取法测定葡萄酒中酯类化合物

Determination of Ester Compounds in Wine Using Dispersive Liquid-Liquid Microextraction

摘要:

为优化分散液液微萃取（dispersive liquid-liquid microextraction，DLLME）测定葡萄酒中酯类化合物的方法，以模拟葡萄酒为试材，研究分散剂种类及体积、萃取剂种类及体积、样品体积、盐添加质量及萃取时间7个因素对模拟葡萄酒中16种酯类化合物萃取效果的影响，结合单因素和Box-Behnken响应面试验对萃取条件进行优化，并采用气相色谱-质谱（GC-MS）进行定性定量分析。结果表明，模拟葡萄酒中酯类化合物的最佳萃取条件为：分散剂甲醇1 200 μL，萃取剂二氯甲烷600 μL，样品体积7 mL，不添加盐，萃取时间1.0 min。在此条件下，16种待测酯类化合物的线性关系良好，R²均高于0.995，检测限（limit of detection，LOD）和定量限（limit of quantitation，LOQ）分别为0.004~0.078 mg/L和0.012~0.261 mg/L；3个质量浓度水平的加标回收率为83.3%~111.3%，日内和日间相对标准偏差（relative standard deviation，RSD）为0.02%~7.69%。对2018—2020年的‘黑比诺’干红葡萄酒和‘贵人香’冰白葡萄酒样品测定时，该方法表现出良好的应用效果，并印证了酯类化合物的种类和质量浓度变化与酒样类型及陈酿年份密切相关。该研究可为深入研究葡萄酒中酯类化合物的代谢提供依据。

Abstract:

To optimize the method for determining ester compounds in wine using dispersive liquid-liquid microextraction (DLLME), a simulated wine solution was used as the test material. The effects of seven factors, including type and volume of dispersant, type and volume of extractant, sample volume, salt addition amount, and extraction time, on the extraction efficiency of 16 ester compounds in simulated wine were investigated. Single-factor experiments and Box-Behnken response surface methodology were combined to optimize the extraction conditions, and qualitative and quantitative analyses were performed using gas chromatography-mass spectrometry (GC-MS). The results showed that the optimal extraction conditions for ester compounds in the simulated wine were 1 200 μL of methanol as the dispersant, 600 μL of dichloromethane as the extraction solvent, a sample volume of 7 mL, no adjustment of ionic strength, and an extraction time of 1.0 min. Under these conditions, all 16 esters compounds under investigation exhibited good linearity with R² exceeding 0.995, while the limits of detection (LOD) and quantitation (LOQ) ranged from 0.004 mg/L to 0.078 mg/L and 0.012 mg/L to 0.261 mg/L, respectively. The spiked recoveries at three mass concentration levels ranged from 83.3% to 111.3%, with intra-day and inter-day relative standard deviations (RSDs) between 0.02% to 7.69%. When applied to ‘Pinot Noir’ dry red wine and Italian ‘Riesling’ ice wine samples from 2018 to 2020, the method showed good applicability, confirming that the types and concentrations of ester compounds were closely related to the wine type and aging year. This study could provide a basis for the in-depth study of the metabolism of ester compounds in wine.