气相色谱法测定自酿葡萄酒中甲醇的含量

目的:针对人们所担忧的葡萄酒中甲醇含量超标的问题,本实验建立一种测定自酿葡萄酒中的甲醇含量的方法。方法:采用气相色谱法对葡萄酒中的杂质甲醇进行定量检测。色谱条件:固定相为Gs BP-Ino WAX毛细管柱,柱温为90℃,载气为氮气,流速为1.4 m L/min;以氢焰离子化检测器（FID）为检测器,温度为200℃;进样口温度为150℃。结果:该方法在16¹000μg/m L的浓度范围内线性关系良好（R2=0.9987）,精密度为1.2%,回收率为90.03%⁹4.00%。结论:该方法快速准确,分析成本低,能够满足快速分析自酿葡萄酒中甲醇的要求。      

自酿葡萄酒在酿造期间甲醇含量控制研究

以常见红葡萄为原料,为控制自酿葡萄酒中甲醇含量,在单因素试验的基础上,选用Box-Behnken响应曲面法对自酿葡萄酒工艺优化。结果表明,选择木质发酵容器,酒曲添加量1.0%,发酵温度24 ℃,发酵时间19 d,陈酿温度20 ℃,陈酿时间81 d为最佳酿造参数。在该酿造工艺条件下,研制所得自酿葡萄酒甲醇含量最低（281 mg/L）,其他各项产品质量指标符合国家相关标准要求。     

葡萄酒,果酒中甲醇含量的气相色谱测定

葡萄酒、果酒中甲醇含量的气相色谱测定刘延琳（西北农业大学葡萄酒学院·陕西杨凌·７１２１００）甲醇（ＣＨ３－ＯＨ）为一元醇，它不是发酵的直接产物，是由天然存在于葡萄酒中的果胶分解而得。甲醇是一种有香气的无色液体，但有毒性。红葡萄酒的甲醇含量为５０－２３...     

气相色谱法测定白酒中杂油醇含量的研究

利用气相色谱（GC）法,建立白酒中杂醇油的测定方法。结果表明,该方法测定杂醇油总量最大偏差为0．161％,重复性、稳定性效果良好,回收率在95％～105％之间,回收率良好,符合要求,表明用此方法测定白酒中杂醇油含量是准确、可行的。     

HS-SPME-GC法测定酿造果酒中甲醇和杂醇的含量

该实验建立并优化了一种顶空固相微萃取-气相色谱法（HS-SPME-GC）检测不同果酒中甲醇和杂醇的研究方法,利用该方法对葡萄酒、山楂酒、猕猴桃酒3种果酒中的甲醇和杂醇含量进行测定,并跟踪测定3种果酒陈酿过程中8种组分的含量变化。结果表明,样品的萃取选择PDMS固相微萃取头,50℃顶空萃取40 min,8种组分采用CP-WAXMS色谱柱（60 m×250μm×0.25μm）分离。在此条件下,各化合物在0.01～50 mg/mL范围内线性关系良好（R>0.999）,检出限为0.001～0.005 mg/mL,定量限为0.003～0.015 mg/mL,加标回收率为88.3%～96.7%,精密度试验结果相对标准偏差（RSD）为2.7%～5.1%。随着陈酿时间的延长,葡萄酒中甲醇含量下降最快,杂醇总量呈增长趋势,而山楂酒、猕猴桃酒的杂醇总量则有不同程度的下降。该方法具有前处理简单、灵敏度高和检测速度快的优点,适用于果酒中甲醇及杂醇含量分析,为其产品质量的评判提供参考。     

气相色谱法测定石榴葡萄酒中的甲醇和杂醇油

以石榴和葡萄为原料榨汁,混合果汁经酸度和糖度调整后(添加蔗糖调整糖度,添加酒石酸和碳酸钙调整酸度),添加酵母,通过前发酵、后发酵,酿制出石榴葡萄酒.再以4-甲基-2-戊醇为内标物,建立了一种可同时测定石榴葡萄酒中甲醇和杂醇油含量的气相色谱测定方法.该方法相对标准偏差为2.1797％～3.2125％,加标回收率为95.8143％～101.9143％,具有较高的精密度和准确度.最后以该方法测定石榴葡萄酒中的甲醇和杂醇油含量,检测结果甲醇未检出,杂醇油(以异丁醇和异戊醇计)0.0228g/100mL.     

葡萄酒中甲醇的气相色谱测定方法的条件优化

本文对葡萄酒中甲醇测定气相色谱分析条件进行探讨,选用ZB-WAX毛细柱、ZB-624毛细柱和GsBP-InoWAX毛细柱三种不同固定液的毛细管柱,对甲醇进行分析,从重现性、柱效、峰形和信噪比等方面进行评价,发现GsBP-InoWAX毛细柱较其他两款毛细柱具有重现性好、柱效高、峰形尖锐,对称性好和信噪比低的优点,筛选出GsBP-InoWAX毛细柱较适合葡萄酒中甲醇气相色谱分析条件。     

自酿葡萄酒生产工艺及过程中的质量控制研究

目的通过对自酿葡萄酒成品进行标准检测及酿酒工艺的危害分析、关键控制点分析,探究各流程对成酒品质的影响,为自酿葡萄酒的质量控制提供理论依据。方法以传统的破碎酿造法手工生产自酿葡萄酒,并按照国家标准对自酿葡萄酒与商业化生产的葡萄酒进行感官、理化及卫生指标检测。结果通过对比检测结果发现,自酿葡萄酒与商业葡萄酒均符合国家规定的检测限值,但自酿葡萄酒的品质较商业葡萄酒仍有一定差距,尤其自酿葡萄酒的挥发酸和甲醇含量较高,分别为1.1 g/L和389 mg.结论自酿葡萄酒酿造过程中产生指标差异的主要原因在于杂菌污染及操作规范2个关键步骤,针对以上问题,本文对自酿葡萄酒的设备及用料质量、发酵过程、贮存及稳定性处理4方面进行了关键点控制。     

蛋白酶对酱香型白酒中杂油醇含量的影响研究

酱香型白酒发酵过程中,研究的蛋白酶添加量对杂油醇生成的影响,结果表明:蛋白酶添加量对杂油醇的生成有一定的影响,在0～20 U/g范围内,杂油醇生成量随蛋白酶添加量的增加而降低,蛋白酶为20 U/g时,杂油醇生成量最低为0.231 g/L,相对于未添加蛋白酶降低60.52%,添加量超过20 U/g时,杂油醇生成量随蛋白酶添加量的增加而增加,各杂油醇单体(异丁醇、正丙醇、异戊醇)变化趋势和总杂油醇变化趋势相似。     

酵母添加量对酱香型白酒中杂油醇影响

杂油醇是白酒中含量较大且对人体有毒害作用,研究不同酵母菌添加量对白酒中杂油醇含量的影响,研究得出:不同酵母添加量对正丁醇、异丁醇、异戊醇及杂油醇总量影响不同,酵母菌添加量1%时,杂醇油的生成量已趋于平缓,且杂油醇生成量较低,和未加酵母菌相比,杂油醇总量降低39.64%。     

Determination of methanol and fusel oils in various types of wines distributed in Korea

Food Science and Biotechnology - The contents of methanol and fusel oils in various types of wines were determined using headspace-gas chromatography (HS-GC). The HS-GC analysis method showed good...     

Major constituents of fusel oils distilled from Australian grape wines

Fusel oils from Australian grape wines (Vine sp. Vitis vinifera) have been found to consist substantially of ethanol, n-propanol, isobutanol (2-methyl-1-propanol), isoamyl alcohol (3-methyl-1-butanol) and active amyl alcohol (2-methyl-1-butanol). In addition there are present large numbers of aliphatic esters, believed to be of considerable importance to grape brandy and spirit flavour and quality. The quantities and occurrence of these esters have been found to follow a systematic pattern. The major esterified alcohols are related to the free alcohols present and the major esterified acids occur as a series of acids of even carbon number with a maximum concentration at the n-decanoic acid. These relationships provide a basis for calculating the approximate ester composition of fusel oil.     

白酒中铅、锰、甲醇、杂醇油含量的测定方法研究

采用原子吸收分光光度法法测定白酒中铅、锰含量,采用将样品低温浓缩蒸发近干后以稀硝酸定容的方法进行前处理,采用外标法定量,线性相关系数R2＞ 0.9990,能力验证实验室间|Z| ≤2.利用气相色谱法同时测定白酒中甲醇和杂醇油含量,采用HP-INNOWAX毛细管柱和氢火焰检测器,外标法定量,能力验证实验室间|Z| ≤2.以上2种检测方法的测定结果均通过由中国国家认证认可监督管理委员会(CNCA)统一组织的能力验证,可以用于测定白酒中铅、锰、甲醇、杂醇油含量,且具有准确、简便、快速的优点.     

Statistical optimization of ethanol fermentation parameters for processing local grape cultivars to wines

Grape juice from two local grape cultivars viz. Punjab MACS purple and H‐144 was subjected to prefermentation skin treatment. Ethanol fermentation w.r.t agitation rate, temperature, inoculum size, and nutrient supplementation were optimized using Triple M medium following response surface methodology (RSM). RSM results were numerically optimized keeping temperature “in range” for red wine and “low” for white wine which showed agitation rate of 80 ± 1 rpm for 24 hr, diammonium hydrogen orthophosphate supplementation @ 150 mg/100 ml, inoculum size of 6.1 and 6.5% (vol/vol), and fermentation temperature of 24.6 and 21 °C as optimum for ethanol fermentation of red and white wines, respectively. Optimized results were validated on grape juice of Punjab MACS purple and H‐144 cultivars that lead to 12.0 and 11.2 (%vol/vol) ethanol production, respectively. Gas chromatography mass spectrometry analysis revealed the presence of 41 volatile compounds in the form of phenols, alcohols, terpenes, esters, ketones, and amines that add to the nutraceutical and antioxidant value of the wines.

Practical applications

Present study provides the statistical optimized fermentation parameters for red and white wine production separately. Optimization of an efficient processing technology to produce local grape wines will help to reduce the price of wines so that they are available to common masses at affordable costs besides improving the economic status of grape growers in the state and providing valuable information to wine makers to establish winery under North Indian conditions. Use of synthetic grape juice (Triple M media; during off season of grapes) lead to optimization of ethanol fermentation parameters in two separate fashions considering fermentation temperature as key parameter. Gas chromatography mass spectrometry analysis showed the presence of flavonoids, terpenes, and esters increasing nutritive value of product, providing antioxidants to the consuming person.     

荔枝酒中杂醇油含量的测定

采用气相色谱法,以叔戊醇为内标物,对荔枝酒中杂醇油的含量进行了测定,并与分光光度法进行了比较分析。实验结果表明,气相色谱法不仅可以检测出荔枝酒杂醇油总量,还能检测出杂醇油组分的含量;荔枝酒中,杂醇油含量较多的成分分别为异戊醇、异丁醇和正丙醇,荔枝干酒中三者含量之和占到杂醇油总量的99.0%;分光光度法是以异丁醇和异戊醇的含量作为杂醇油总量,该法无法检测到荔枝酒中正丙醇的含量,不能准确测定荔枝酒中杂醇油含量,气相色谱法具有简单、快速、精密度高等特点,较分光光度法更适合于荔枝酒中杂醇油含量的测定。     

白酒中杂醇油测定误差的原因及改进措施

测定白酒中杂醇油常采用硫酸-对二甲胺基苯甲醛比色法，但测定常有误差。通过反复实验对杂醇油测定过程中出现的误差原因进行了分析、提出了改进措施。     

发酵温度对浓香型白酒杂醇油含量的影响

为探究发酵温度对浓香型白酒生产中杂醇油生成量的影响,该研究利用可实现夹套控温的固态发酵罐为发酵容器,分别进行两轮“控温发酵”实验,对控温发酵罐、未控温发酵罐（对照）和窖池发酵过程中糟醅中及基酒中的杂醇油进行对比分析。结果表明,通过控制固态发酵罐夹层水温可有效实现对发酵糟醅温度的控制,且第一轮控温后与对照罐（32.4 ℃）相比,控温后顶温（35 ℃）更高,中挺时间更长（13 d）;第二轮控温后发酵罐糟醅形成了2 ℃以上的温差,温度较高的发酵罐中挺时间较长（15 d）;经气相色谱分析检测发酵温度较高的发酵罐,其糟醅中正丙醇、异丁醇、正丁醇、异戊醇、正己醇等杂醇油含量增加了118.6%、21.2%、29.7%、21.7%、77.3%,其二段基酒中正丙醇、正丁醇、异戊醇、正己醇等杂醇油含量也较发酵温度较低的发酵罐高22.3%、0.6%、2.0%、25.4%。     

比色法测葡萄酒中杂醇油含量的方法优化

蒸馏酒及配制酒中杂醇油的测定常用硫酸-对二甲胺基苯甲醛比色法.此方法以化学分析为基础,操作简单,实验条件的要求较低,但此方法显色不稳定,测定常有误差.该文通过研究比色法测定葡萄酒中杂醇油含量的实验条件,得出了一种稳定性良好、准确度高的实验方法.即酒样经过预处理后,显色剂浓度选择5g/L的对二甲胺基苯甲醛-硫酸溶液,在80℃水浴30min,稀释剂选择2mL硫酸溶液,于波长520hm处测定吸光度值.     

Ochratoxin A in wines,musts and grape juices from Spain

A survey on the occurrence of ochratoxin A (OTA) in 240 grape‐based beverages was carried out. Red and white wines from four different Spanish Designations of Origin (n = 160), musts (n = 20), grape juices (n = 10), ordinary wines (n = 20), special wines (Malaga, muscatel, sherry, vermouth, etc) (n = 20) and sparkling wines (n = 10) were assayed for OTA content using immunoaffinity column clean‐up and high‐performance liquid chromatography with fluorimetric detection (detection limit 0.05 µg l^?1). Forty‐three (17.9%) of the samples tested contained detectable levels of OTA. The overall mean OTA concentration in red and white wines of Designations of Origin was 0.30 and 0.18 µg l^?1 respectively (ranges 0.05–3.19 and 0.05–1.13 µg l^?1 respectively). The percentage of wine samples with detectable amounts of OTA was higher for red (18.3%) than for white (10%) wines. OTA was also found in two of 10 red ordinary wines (0.68 and 4.24 µg l^?1), whereas none of 10 white ordinary wines contained OTA. The mean OTA amount detected in sparkling wines was 0.44 µg l^?1 (range 0.14–0.71 µg l^?1). Two of 20 must samples contained OTA at low levels (0.08 and 0.18 µg l^?1), while none of 10 grape juice samples contained OTA. Highest amounts of OTA were found in special wines (45%), with a maximum of 15.25 µg l^?1 in a muscatel sample. Copyright © 2004 Society of Chemical Industry