活性炭吸附塑化剂后白酒品质的变化

发布时间：2018-01-16 16:31

本文关键词：活性炭吸附塑化剂后白酒品质的变化　出处：《沈阳农业大学》2017年硕士论文　论文类型：学位论文

【摘要】：白酒是我国重要产业之一,"酒鬼"酒的事件对我国的白酒行业带来了巨大的冲击,此次事件使众多消费者对白酒中的塑化剂的有着高度的关注。目前,国内外研究较多是针对于白酒中塑化剂的来源、检测方法与去除方法等,但对活性炭脱除塑化剂及其对白酒品质影响的相关报道很少。本试验的目的就是在实验室的条件下,研究使用活性炭吸附后白酒理化品质的变化,尤其是香气物质的变化,并根据塑化剂脱除效果和脱塑后白酒的理化品质等指标,选取出一种较好的活性炭。本文参照国标中的检测方法,建立了白酒中塑化剂的GC-MS检测方法,将得到的16种邻苯二甲酸酯标准品的谱图与定性参数结合NIST11.L谱库进行比对作为定性标准;外标法作为定量方法,根据其检测数据绘制出16种塑化剂的标准曲线,该方法的R2在0.9981～0.9996之间,16个组分在线性范围内的相关系数良好,其检出限在0.047μg/kg～1.999μg/kg之间,定量限在0.155μg/kg～6.662μg/kg之间,回收率在77.7%～108.4%之间,而相对偏差在1.9%～8.3%之间。在浓香型白酒中检测出4种塑化剂,但其经过活性炭T1、T2吸附后,检出量大多低于其检出限,所以在之后的试验中不以浓香型白酒作为试验对象。从酱香型白酒中检测出8种塑化剂,其中现已发布的有限量规定的邻苯二甲酸二正丁酯(DBP)和邻苯二甲酸二(2-乙基己)酯(DEHP)的含量略高于其标准,经活性炭T1、T2脱除后,均已符合限量规定,且脱除率高达70%以上,其余6种塑化剂经过活性炭T1脱除后,脱除率都高于65%,经过活性炭T2脱除后检出量都低于其检出限,所以活性炭T1和T2对酱香型白酒中塑化剂都有良好的吸附效果,且活性炭T2的吸附效果优于活性炭T1。本文采用指示剂法与比色法对活性炭吸附前后酱香型白酒的理化品质进行研究。总酸总酯的试验结果参考国标GB/T 26760-2011和GB/T 10781.1-2006,酱香型白酒吸附由结果可知活性炭的吸附会对白酒理化性质中总酸总酯与甲醇含量造成一定的损失,并以总酸总酯与甲醇损失量为标准,参考方差分析结果,可知活性炭T1和T2对总酸总酯与甲醇的吸附效果的差异显著;对糠醛和杂醇油吸附效果的差异并不显著。所以,活性炭T2对酱香型白酒中的总酸总酯、甲醇、杂醇油与糠醛的吸附性要优于活性炭T1;而对于杂醇油和糠醛两种活性炭的吸附效果差异并不明显,故综合各理化指标结果,选取活性炭T1作为脱除活性炭的效果较好。运用固相微萃取法检测出44种香气物质,而液-液萃取法中却检测出了 65种香气物质,但其中有29种香气物质在两种前处理方法中均检出;并且在仅用各方法单独检出的香气成分中,液-液萃取法中检测出了在酱香型白酒中含量较高且重要的香气物质乳酸乙酯、乙酸乙酯和乳酸等,并且在液-液萃取法中所检测出的香气成分的种类也多于固相微萃取法。运用活性炭T1吸附酱香型白酒后,共检测出48种香气物质,有17种香气物质未检出,而使用活性炭T2吸附后,共检测出37种香气物质,有28种香气物质未检出。活性炭T1吸附后的香气物质损失率普遍低于50%,活性炭T1吸附后的香气物质损失率普遍高于50%;且在酱香型白酒中较为重要且相对含量较高的化合物经活性炭T2吸附的损失率均是活性炭T1吸附的损失率4倍以上。综上所述,活性炭虽然对白酒中的塑化剂有良好的去除作用,但是也造成了白酒中其它成分的损失,尤其是作为判断白酒品质的重要指标之一的香气成分;活性炭T2因其接触表面积大于活性炭T1,对物质的吸附效果也要好于活性炭T1,但是同样的总酸总酯与香气物质的损失也要高于活性炭T1。故以两种活性炭对塑化剂的脱除效果以及各理化品质的吸附状况为指标,选取活性炭T1作为脱除酱香型白酒中塑化剂的吸附剂。
[Abstract]:The liquor is one of the most important industries in our country, "alcoholic" events of China's liquor industry has brought great impact on the incident, so that many consumers of the liquor plasticizing agent has a high degree of attention. At present, the domestic and foreign research more is the source for the liquor plasticizer, detection and removal methods etc. However, reports on activated carbon removal and its effect on the quality of liquor plasticizer rarely. The purpose of this experiment is under laboratory conditions, changes of active carbon absorption liquor after the physicochemical quality, especially the changes of aroma substances, and the removal effect and removal of plasticizer according to physicochemical quality of liquor after the plastic and select a better activated carbon. According to the detection method in the national standard, established GC-MS detection method of liquor plasticizer, the 16 kinds of phthalate two formic acid ester standard spectrum and Parameters combined with NIST11.L database to compare as qualitative criteria; external standard method for quantitative methods, according to the detection data drawing standard curve of 16 kinds of plasticizer, the method of R2 in 0.9981 ~ 0.9996, the correlation coefficient of 16 components in linear range, the detection limit at 0.047 g/kg ~ 1.999 g/kg, the limit of quantification between 0.155 g/kg ~ 6.662 g/kg, the recovery was 77.7% ~ 108.4%, and the relative deviation in 1.9% ~ 8.3%. Detected 4 kinds of plasticizer in Luzhou flavor liquor, but the activated carbon after T1, T2 after adsorption, mostly below the detection limit of detection. So after the test is not in Luzhou flavor liquor as the test object. To detect 8 kinds of plasticizer from Maotai liquor, which has released a limited amount of the provisions of the two butyl phthalate two formic acid (DBP) and the adjacent benzene two formic acid two (2- ethylhexyl) ester (DEHP) content slightly The higher standard, T1 removal by activated carbon, T2, are in line with limited provisions, and the removal rate is more than 70%, the remaining 6 kinds of plasticizer activated carbon after T1 removal, the removal rate is higher than 65%, activated carbon after removal of T2 after the detection amount is lower than the detection limit, so the activated carbon T1 and T2 the plasticizer in Maotai flavor liquor has good adsorption effect of activated carbon, and the adsorption of T2 is better than that of activated carbon by T1. indicator method and colorimetric method for adsorption of activated carbon before and after physical and chemical quality of Maotai flavor liquor were studied. The test results of total acids and total esters of GB GB/T 26760-2011 and GB/T 10781.1-2006 reference, Maotai the results indicated that liquor adsorption of activated carbon will be the white wine physicochemical properties in total acid and total ester content of methanol and caused some losses, and the total acids and total esters and methanol loss as the standard, the results showed that the active carbon reference variance, T1 and T2 The difference of adsorption effect of total acids and total esters with methanol significantly; the difference of furfural and fusel oil adsorption effect is not significant. So, the activated carbon T2 on total acids and total esters, Maotai liquor in the methanol, adsorption of fusel oil and furfural was superior to that of activated carbon T1; and for the difference of adsorption effect of fusel oil furfural and two kinds of activated carbon is not obvious, so the physicochemical index results, select the activated carbon T1 as active carbon removal effect is good. The use of solid phase micro extraction method to detect 44 kinds of aroma substances, and liquid-liquid extraction was detected in 65 kinds of aroma substances, but there are 29 kinds of aroma the material in the two pretreatment methods were detected; and in aroma components only detected by the method of liquid-liquid extraction method detected the aroma of ethyl lactate in Maotai liquor was higher and important, ethyl acetate and lactate, and in The types of aroma components detected by liquid-liquid extraction method in the more solid phase micro extraction. Using activated carbon adsorption T1 of Maotai liquor, detected a total of 48 aroma substances, there are 17 kinds of aroma substances were not detected, and the use of activated carbon adsorption of T2, detected a total of 37 kinds of aroma substances, have 28 kinds of aroma substances were not detected. T1 activated carbon adsorption aroma loss rate is generally lower than 50%, activated carbon adsorption and T1 the aroma loss rate is generally higher than 50%; and in Maotai liquor is an important and relatively high content of compounds by activated carbon adsorption T2 loss rate are T1 active carbon adsorption the loss rate of more than 4 times. In conclusion, although the activated carbon has good removing effect of plasticizer in liquor, but also caused the loss of other ingredients in liquor, especially as an important index of judging the aroma components of wine quality; active carbon T2 Because the contact surface area greater than T1 on the adsorption of activated carbon, activated carbon material is better than T1, but the total acid and ester aroma substances and the same loss is higher than that of activated carbon T1. so to two kinds of activated carbon on the removal effect of plasticizer and the Physicochemical Quality of the adsorption condition as the index selection activity carbon T1 as adsorbent for removal of plasticizer in Maotai flavor liquor.

【学位授予单位】：沈阳农业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS262.3

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