高效液相色谱法测定黄酒中的β-苯乙醇

建立一种采用反相高效液相色谱法测定黄酒中β- 苯乙醇的方法。采用反相C18 色谱柱Synergi Hrdro-RP C18(4.6mm × 250mm,4μm),以甲醇- 水为流动相(50:50,V/V),流速1ml/min,紫外检测器,检测波长210nm,对黄酒中的β- 苯乙醇进行检测。结果表明,在5.00～30.00mg/L 添加量范围内,回收率水平在99.5%～99.8% 之间,相对标准偏差为0.6% (n = 6),方法的检出限为0.05mg/L,线性范围为0.5～50mg/L(r = 0.9999),测定结果与标准气相色谱方法基本相同。所建立的方法可以作为黄酒中β- 苯乙醇的检测方法。     

反相高效液相色谱法测定黄酒中的草酸

该文建立了一种利用反相高效液相色谱法测定黄酒中草酸的方法,该方法以邻苯二胺为衍生剂,在高温酸性条件下与草酸反应,生成强紫外吸收化合物——2,3-二羟基喹喔啉,对其检测的最优色谱条件是:Dionex Acclaim 120 C18柱(4.6×250 mm,5μm);以甲醇和0.1mol/L乙酸铵(15:85 v/v)为流动相;流速1.2mL/min;检测波长314nm;柱温25℃。该方法测定黄酒样品中草酸的回收率为91.40%~103.70%,相对标准偏差小于9.30%。该方法简便、准确,适合测定黄酒中草酸的含量。     

Simultaneous Determination of 15 Phenolic Constituents of Chinese Black Rice Wine by HPLC‐MS/MS with SPE

This study established a new method for quantitative and qualitative determination of certain components in black rice wine, a traditional Chinese brewed wine. Specifically, we combined solid‐phase extraction and high‐performance liquid chromatography (HPLC) with triple quadrupole mass spectrometry (MS/MS) to determine 8 phenolic acids, 3 flavonols, and 4 anthocyanins in black rice wine. First, we clean samples with OASIS HLB cartridges and optimized extraction parameters. Next, we performed separation on a SHIM‐PACK XR‐ODS column (I.D. 3.0 mm × 75 mm, 2.2 μm particle size) with a gradient elution of 50% aqueous acetonitrile (V/V) and water, both containing 0.2% formic acid. We used multiple‐reaction monitoring scanning for quantification, with switching electrospray ion source polarity between positive and negative modes in a single chromatographic run. We detected 15 phenolic compounds properly within 38 min under optimized conditions. Limits of detection ranged from 0.008 to 0.030 mg/L, and average recoveries ranged from 60.8 to 103.1% with relative standard deviation ≤8.6%. We validated the method and found it to be sensitive and reliable for quantifying phenolic compounds in rice wine matrices.     

酶标仪比色法检测浊米酒中高级醇含量

为探索酶标仪比色法在浊米酒高级醇含量检测中的适用性,该研究建立了酶标仪比色法检测浊米酒中6种高级醇(异丁醇、异戊醇、苯乙醇、正丙醇、正丁醇、己醇)的单一和混合标准曲线,并对比了酶标仪比色法和气相色谱法对浊米酒中高级醇含量的检测效果。结果表明,酶标仪比色法建立的混合标曲在0~0.05 mg线性均较好,单一标曲中正丙醇在0~1 mg线性较差,而苯乙醇和正丁醇在0~0.05 mg线性稍差,并在一定程度上影响其他高级醇检测效果;酶标仪比色法测得FBKL2.8022和FBKL2.8023发酵米酒中6种高级醇的质量浓度分别为408.94 mg/L和230.89 mg/L,其中6种高级醇含量的标准偏差分别为0.06%~3.94%和0.72%~1.58%,酶标仪比色法测定结果高于气相色谱法。该研究使用酶标仪比色法检测发酵米酒中不同高级醇的含量,发现高级醇配比不同会影响标准曲线的线性方程和相关系数,因此需要根据样品检测需求而选择合适配比的标曲进行样品检测分析。     

Optimization of fermentation conditions for Chinese bayberry wine by response surface methodology and its qualities

Colour and flavour are both important challenges for bayberry wine production because of a shortage of selected strains. The yeast Saccharomyces cerevisiae strain YF152, separated from a natural Chinese bayberry fermentation mash [alcohol tolerance capacity (18.0%), SO₂ (200 mg/L), sugar content (40%) and pH (2.50)] was employed to brew Chinese bayberry wine. Response surface methodology was used to simultaneously analyse the effects of the fermentation conditions on Chinese bayberry wine. The optimum conditions were found to be a temperature of 26.5 °C, an initial sugar content of 22.0°Brix, an inoculum size of 4.0% and an initial pH of 2.90. Under these conditions, the final alcohol content of the bayberry wine was 13.4%, the anthocyanin content was 77 mg/L and the residual sugar content was 1 g/L. These numbers agreed well with the predicted values. The major characteristic flavour components of the wine were 3‐methyl‐1‐butanol, 2‐phenylethanol, ethyl acetate, 2‐methylbutyl acetate and acetic acid. Copyright © 2016 The Institute of Brewing & Distilling     

Effect of γ‐aminobutyric acid supplementation on the composition of Chinese rice wine

This study investigated the effect of γ‐aminobutyric acid (GABA) supplementation on the composition of Chinese rice wine. GABA was added at 188.5 and 377 mg/L at the beginning of primary fermentation or post‐fermentation. Addition of GABA during primary fermentation had no impact on alcohol and total acid formation or the utilisation of sugar. However, total free amino acids, total essential amino acids and GABA in rice wine supplemented with GABA were significantly lower than the control rice wine without supplementation. Alcohol formation, total acid, sugar content and total essential amino acids were similar compared with the control. However, the GABA post‐supplementation was significantly higher, suggesting that GABA supplementation post‐fermentation process could enhance the GABA content in rice wine. © 2018 The Institute of Brewing & Distilling     

Characterization of Volatile and Semi‐Volatile Compounds in Chinese Rice Wines by Headspace Solid Phase Microextraction Followed by Gas Chromatography‐Mass Spectrometry

The volatile and semi‐volatile compounds of Chinese rice wines were extracted by headspace solid phase microextraction (HS‐SPME) and analyzed by gas chromatography‐mass spectrum (GC‐MS). The original Chinese rice wine samples were diluted with deionized water to a final concentration of 6% (v/v) ethanol and then extracted by HS‐SPME. The samples were pre‐equilibrated at 50°C for 15 min and extracted with stirring at the same temperature for 45 min prior to injection into a GC‐MS. A total of 97 volatile and semi‐volatile compounds were identified from ten Chinese typical rice wine samples, including 13 alcohols, 8 acids, 28 esters, 4 aldehydes and ketones, 17 aromatic compounds, 3 lactones, 6 phenols, 3 sulphides, 9 furans and 6 nitrogen‐containing compounds, of which, 39 compounds were firstly reported in Chinese rice wine. By stepwise linear discrimination analysis, the ten Chinese rice wine samples could be classified into three groups according to the production area, and in particular, the production technologies.     

黄酒中9 种生物胺的高效液相色谱分析法

建立一种检测黄酒中生物胺的反相高效液相色谱法。用三氯乙酸提取黄酒中生物胺,丹磺酰氯作为衍生化试剂,1,7-二氨基庚烷作为内标定量。色谱条件为：Waters XBridge C18色谱柱（4.5 mm×250 mm,3.8 μm）作为分离柱,乙腈和水作为流动相进行梯度洗脱,流速1 mL/min,紫外检测波长254 nm。结果表明,9 种生物胺（盐酸吡哆胺、色胺、腐胺、尸胺、β-苯乙胺、组胺、酪胺、精胺和亚精胺）在40 min内能被很好分离。在1～50 mg/L质量浓度范围内,各种生物胺呈现良好的线性相关性（R2＞0.999）。各生物胺加标回收率为79.54%～89.55%,相对标准偏差为3.14%～6.35%,该法各组分检出限（RSN=3）为0.002～0.009 mg/L。应用柱前衍生化高效液相色谱-紫外检测法,实现了黄酒中生物胺的准确检测。     

Phenolics,Aroma Profile,and In Vitro Antioxidant Activity of Italian Dessert Passito Wine from Saracena (Italy)

A traditional sweet dessert wine from Saracena (Italy), made with nonmacerated local white grapes (Guarnaccia, Malvasia and Moscato), was analyzed for phenolics and aroma profile and antioxidant activities. The most abundant classes of phenols identified by high‐performance liquid chromatography were hydroxybenzoic acids and flavan‐3‐ols, where gallic acid showed the highest content (376.5 mg/L). The analysis by solid phase microextraction‐gas chromatography‐mass spectrometry revealed the presence of superior alcohols (from iso‐butanol and iso‐amyl alcohol up to 2‐phenylethanol) and their ethyl esters, terpenes (such as linalool), furfuryl compounds, and free fatty acids (up to palmitic acid) as the key odorants of this wine. The antioxidant activity, evaluated by different in vitro assays 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH), 2,2′‐azino‐bis(3‐ethylbenzothiazoline‐6‐sulphonic acid (ABTS), and β‐carotene bleaching test), showed that passito wine had a radical scavenging activity (IC₅₀ value of 0.03 v/v against DPPH·) and inhibited linoleic acid oxidation with an IC₅₀ value of 0.4 v/v after 30 min of incubation.     

Mango wine aroma enhancement by pulp contact and β‐glucosidase

This study determined the influence of pulp maceration and β‐glucosidase on mango wine physico‐chemical properties and volatile profiles. The distinction in pH, sugars and organic acids among different treatments was not statistically significant. All wine samples reached around 8% (v/v) ethanol from about 16% (w/v) of sugars. The wine with pulp contact contained about ten times higher α‐terpinolene and up to three times higher acetate esters than the wine without pulp contact, but mitigated the production of medium‐chain fatty acids and relative ethyl esters by up to six times. β‐glucosidase enhanced terpenols by up to ten times and acetate esters by up to three times. Furthermore, enzyme treatment mitigated, by up to five times, the formation of medium‐chain fatty acids and ethyl esters to moderate levels. Sensory evaluation showed pulp contact, and β‐glucosidase not only improved the intensity and complexity of wine aroma but balanced odour attributes.     

黄酒中氨基甲酸乙酯直接减除技术的研究

黄酒中含有微量氨基甲酸乙酯(Ethyl Carbamate),简称EC,直接降低黄酒中的EC含量,具有重要的现实意义。在各种吸附性材料中,优选得特异性功能树脂材料L2、L3,复配后以合适的添加量体积分数10%处理酒样,对黄酒中的EC能较有效减除,去除率在60%以上,基本达到EC限量要求,同时对酒体风味的保持较好。材料对EC的减除为吸热过程,实际应用中需保证作用温度大于20℃。面向中国黄酒中EC含量的直接降低,提供了一个实用、便捷的全新途径。     

不同类型黄酒中杂醇油含量分析及其机制初探

杂醇油是引起黄酒上头的主要因素,严重影响黄酒的品质。该研究建立了外标法顶空进样毛细管气相色谱法测定清爽型黄酒中杂醇油的方法。结果表明方法准确可靠,线性范围为0～1 000 mg/L,样品加标回收率均大于96%,相关系数大于0.998 8,相对标准偏差为1.09%～1.72%。利用该法检测了市场上常见的10种黄酒,结果表明,杂醇油含量最高为528.4 mg/L,最低为152.8 mg/L。杂醇油含量按类型呈现干型<半干型≈半甜型<甜型的特征,初步探明不同工艺会导致黄酒中杂醇油含量的差异。最后通过与其它酒种的比较证实杂醇油是影响黄酒品质的重要因素。     

Determination of γ‐aminobutyric acid in Chinese rice wines and its evolution during fermentation

γ‐Aminobutyric acid (GABA) is a functional amino acid that is widely present in Chinese rice wine. In this study, high‐performance liquid chromatography coupled with ultraviolet detection (HPLC‐UV) was established for the determination of γ‐aminobutyric acid in 22 Chinese rice wines collected from the Shaoxing region of China. Furthermore, the evolution of GABA was studied in Chinese rice wine during primary and post‐fermentation process. Results showed that the HPLC method was reliable with good linearity, accuracy, precision and stability. Additionally, the GABA content varied significantly in the 22 Chinese rice wines, and the content was much higher in wine samples with long aging periods. Regarding the evolution of GABA in Chinese rice wine during the brewing process, the level slowly increased during primary fermentation. A decrease in GABA was observed in the wine at the early stage of the post‐fermentation process. However, a marked increase on the GABA content occurred in wine at the late stage of post‐fermentation. The findings from this study are that HPLC can be successfully applied to determine GABA in Shaoxing brewed rice wines, and further provide useful information on quality control of such wines. Copyright © 2017 The Institute of Brewing & Distilling     

含Monacolin K黄酒的酿造及成分分析

利用含有Monacolin K麦曲进行含有Monacolin K黄酒的酿造,实验黄酒的酿造配方并对黄酒成品进行成分分析。确定黄酒的酿造配方,感官质量符合黄酒国家标准;产品成分分析表明:该黄酒总糖(以葡萄糖计)含量为26.1 g/L,酒精度为15.6%(v/v),总酸含量为5.1 g/L(以乳酸计),Monacolin K含量为0.080 mg/mL,pH值为4.1,氨基态氮含量为0.58 g/L,含有人体所必需的各种氨基酸。     

麻城老米酒中酚类物质的初探

以糯米为主要原料,进行半固态发酵得到麻城老米酒,采用高效液相色谱（HPLC）法对麻城老米酒中酚类物质进行定性定量分析,色谱条件为Hypersil Gold C18 色谱柱（250 mm×4.6 mm,5 μm）用作分离柱,0.1%的甲酸水和甲醇用作梯度洗脱的流动相,流速1 mL/min,紫外检测波长280 nm;结果表明,方法的检出限为0.117～0.156 mg/L,回收率均在86.2%～102.3%,相对标准偏差（RSD）为0.48%～2.75%。该方法检测了麻城老米酒中11种酚类物质,其中儿茶素、表儿茶素、芦丁是老米酒中主要的单酚物质,占总含量的比例较大。     

PITC柱前衍生-反相高效液相色谱法测定黄酒中游离氨基酸和生物胺

建立柱前衍生-反相高效液相色谱,同时测定黄酒中17 种氨基酸及7 种生物胺含量的方法。采用异硫氰酸苯酯柱前衍生试剂,采用Inertsil ODS-SP C18（250 mm×4.6 mm,5 μm）分析,以乙酸钠溶液和乙腈溶液混合液进行梯度洗脱,在254 nm波长处进行氨基酸和生物胺的含量分析。氨基酸和生物胺在2.0～500 mg/L和0.5～125 mg/L范围内具有良好的线性关系,相关系数R2大于0.99,平均回收率在86.44%～99.75%之间,相对标准偏差在0.31%～3.53%之间;检出限为0.02～0.25 mg/L,定量限为0.25～4.50 mg/L。方法线性范围广、准确性高、稳定性好,适用于黄酒中氨基酸及生物胺的检测。     

Fatty acids and all‐trans‐β‐carotene are correlated in differently colored rice landraces

A set of 54 rice landrace samples was compiled from various Asian countries, including six red/brownish and eight black/purple varieties. Brown rice samples were analyzed for lipid content and fatty acid profile, as well as all‐trans‐β‐carotene content. Black/purple varieties were found to be higher in crude lipid content than the red/brownish and colorless varieties. They also had a higher β‐carotene content than the other two color classes. The highest β‐carotene content determined was 0.22 mg kg⁻¹. Black/purple varieties tended to have a higher proportion of saturated fatty acids in their lipid fraction and a lower proportion of unsaturated fatty acids. The differences were statistically significant (P < 0.05) for oleic acid, which accounted for 42.1% of the lipid fraction in black/purple varieties and for 45.3% and 46.3% in red/brownish and colorless varieties, respectively. β‐Carotene content showed a significantly positive correlation with the crude lipid content (P < 0.001) and the content of saturated fatty acids (P < 0.001) on a dry matter basis. However, it was not correlated with the unsaturated fatty acids content on a dry matter basis. Within the total lipid extract, β‐carotene showed a significantly positive correlation with the proportion of saturated fatty acids (P < 0.01), especially palmitic acid (P < 0.01), and a significantly negative correlation with unsaturated fatty acids (P < 0.001), especially oleic acid (P < 0.01). Copyright © 2005 Society of Chemical Industry     

炭黑氨基柱净化HPLC-ICP-MS测定黄酒中砷形态及含量

建立了一种同时测定黄酒中亚砷酸根、砷酸根、砷甜菜碱、一甲基砷酸和二甲基砷酸等5种砷形态的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。黄酒经炭黑氨基柱净化,体积分数为10%甲醇水溶液洗脱,采用Hamilton PRP-XIO0阴离子交换色谱柱(4.1 mm×250 mm,10 μm),60 mmol/L硝酸铵梯度洗脱,高效液相色谱分离,电感耦合等离子体质谱进行定性和定量分析。在0.5～20.0 μg/L范围内各砷形态线性良好,相关系数R均＞0.999;加标回收率85%～92%,相对标准偏差(RSD)1.4%～5.2%;5种砷形态的定量限均为0.10 μg/L,检出限均为0.03 μg/L。利用该方法对不同年份、不同企业及不同类型的黄酒进行了检测,该方法适用于黄酒中砷残留的分析检测。     

发酵型饮料酒中生物胺含量的调查与分析

利用反相高效液相色谱技术,以丹磺酰氯柱前衍生,分析了我国市场中32个啤酒样品、32个葡萄酒样品和12个黄酒样品中生物胺的含量。结果表明,我国啤酒、葡萄酒样品中含有较低的生物胺物质,平均含量分别为4.787 mg/L和11.240 mg/L,黄酒中生物胺含量较高,达到了78.304 mg/L。3种饮料酒含量较多的单体生物胺均为腐胺和酪胺,我国葡萄酒中的组胺含量低于国际现有组胺标准的最低限量要求。不同企业生产的啤酒样品和不同原产地的葡萄酒样品中组胺含量存在显著差异,黄酒样品中生物胺含量为18.603～140.010 mg/L,样品间差异很大。     

HPLC determination of γ‐aminobutyric acid in Chinese rice wine using pre‐column derivatization

γ‐Aminobutyric acid (GABA) is a major functional ingredient in Chinese rice wine. A new HPLC method for determining GABA using pre‐column derivatization with dansyl chloride was developed. The HPLC operating conditions were as follows: a Hypersil ODS2 C₁₈ column; mobile phase, methanol and water (1:1); gradient elution; absorption at 254 nm; flow rate, 1 mL/min; pH 9; and column temperature, 30 °C. Under optimal HPLC conditions, the linear equation was y = 3.5 × 10^?7x ? 0.014. The precision (relative standard deviation, RSD) was 0.54%, the stability (RSD) was 0.21%, the recovery ratio was 97.4% and reproducibility (RSD) was 1.57%. This new method appears to be sensitive, accurate, convenient, steady and relatively fast. The results suggest that the new method is also more reliable. Copyright © 2015 The Institute of Brewing & Distilling