Debebe Ayalew, Redi-Abshiro Mesfin, Chandravanshi Bhagwan Singh
Department of Chemistry, Addis Ababa University, P.O. Box 1176, Addis Ababa, Ethiopia.
Department of Chemistry, Haramaya University, P.O. Box 138, Dire Dawa, Ethiopia.
Chem Cent J. 2017 Mar 24;11(1):27. doi: 10.1186/s13065-017-0257-5.
Traditional fermented alcoholic beverages are indigenous to a particular area and are prepared by the local people using an age-old techniques and locally available raw materials. The main objective of this work was the direct determination of ethanol in traditional fermented alcoholic beverages using mid infrared spectroscopy with partial least squares regression, verifying the robustness of the calibration models and to assess the quality of beverages.
The level of ethanol determination in Ethiopian traditional fermented alcoholic beverages was done using mid infrared spectroscopy with partial least squares regression (MIR-PLS). The calibration and validation sets, and real samples spectra were collected with 32 scans from 850-1200 cm. A total of 25 synthetic standards (calibration and validation sets) with ethanol (2-10% w/w) and sugars (glucose, fructose, sucrose and maltose) (0-5% w/w) compositions were used to construct and validate the models. Twenty-five different calibration models were validated by cross-validation approach with 25 left out standards. A large number of pre-treatments were verified, but the best pre-treatment was subtracting minimum + 2nd derivative. The model was found to have the highest coefficients of determination for calibration and cross-validation (0.999, 0.999) and root mean square error of prediction [0.1% (w/w)]. For practical relevance, the MIR-PLS predicted values were compared against the values determined by gas chromatography. The predicted values of the model were found to be in excellent agreement with gas chromatographic measurements. In addition, recovery test was conducted with spiking 2.4-6.4% (w/w) ethanol. Based on the obtained recovery percentage, 85.4-107% (w/w), the matrix effects of the samples were not considerable.
The proposed technique, MIR-PLS at 1200-850 cm spectral region was found appropriate to quantify ethanol in fermented alcoholic beverages. Among the studied beverages (Tella, Netch Tella, Filter Tella, Korefe, Keribo, Borde and Birz), the average ethanol contents ranged from 0.77-9.1% (v/v). Tej was found to have the highest ethanol content whereas Keribo had the least ethanol content. The developed method was simple, fast, precise and accurate. Moreover, no sample preparation was required at all. However, it should be noted that the present procedure is probably not usable for regulatory purposes (e.g. controlling labelling).
传统发酵酒精饮料原产于特定地区,由当地居民使用古老技术和当地可得原料酿制而成。本研究的主要目的是利用中红外光谱结合偏最小二乘法回归直接测定传统发酵酒精饮料中的乙醇含量,验证校准模型的稳健性并评估饮料质量。
采用中红外光谱结合偏最小二乘法回归(MIR-PLS)测定埃塞俄比亚传统发酵酒精饮料中的乙醇含量。校准集、验证集和实际样品光谱在850 - 1200 cm范围内进行32次扫描采集。共使用25种含有乙醇(2 - 10% w/w)和糖类(葡萄糖、果糖、蔗糖和麦芽糖)(0 - 5% w/w)成分的合成标准品(校准集和验证集)构建并验证模型。通过留一法对25种不同的校准模型进行交叉验证。对大量预处理方法进行了验证,最佳预处理方法是减去最小值 + 二阶导数。该模型在校准和交叉验证中的决定系数最高(0.999,0.999),预测均方根误差为[0.1%(w/w)]。为了实际应用,将MIR-PLS预测值与气相色谱法测定值进行比较。发现该模型的预测值与气相色谱测量值高度吻合。此外,进行了添加2.4 - 6.4%(w/w)乙醇的回收率试验。根据获得的回收率85.4 - 107%(w/w),样品的基质效应不显著。
所提出的1200 - 850 cm光谱区域的MIR-PLS技术适用于定量发酵酒精饮料中的乙醇。在所研究的饮料(泰拉、内奇泰拉、过滤泰拉、科雷费、凯里博、博尔德和比尔兹)中,乙醇平均含量范围为0.77 - 9.1%(v/v)。泰吉的乙醇含量最高,而凯里博的乙醇含量最低。所开发的方法简单、快速、精确且准确。此外,完全无需样品制备。然而,应当指出,本方法可能不适用于监管目的(如控制标签)。