高效液相色谱法测定罗城“桂葡1号”毛葡萄酿酒过程中9种酚类物质的变化

Content Changes of 9 Phenolic Compounds during the Fermentation of Luocheng“Gui-pu No.1”Vitis quinnquangularis Rehd Wine Traced by HPLC

为给毛葡萄酒优质化酿造提供技术支持,开发了9种代表性酚类物质的定量方法,并跟踪了其发酵过程的变化。通过波长和梯度优化确定色谱条件为:Atlanis T3色谱柱(4.6 mm×250 mm,5μm),流速1 mL/min,梯度洗脱,柱温30℃,检测波长280、306、320、360 nm,上样量10μL。该方法线性范围较宽,R2>0.989,定量限0.056~0.987 mg/L,混合标样梯度4对应的加标回收率92.37%~103.45%,相对标准偏差≤3.26%。对“桂葡1号”毛葡萄在22℃和28℃发酵过程中的酚类物质变化进行跟踪,结果表明:只有山奈酚在初始发酵液中无检出;不同酚类物质的含量变化趋势不同;除虎杖苷和绿原酸在发酵过程中一直下降外,其它酚类物质均呈先升后降的趋势;各物质在两个发酵温度下的变化趋势基本一致,只是幅度不同;在两个发酵温度对应的15 d发酵液中,只有矢车菊素-3-O-葡萄糖苷、山奈酚、阿魏酸的含量均高于初始发酵液的含量。该研究为毛葡萄酒酚类物质的品控提供了有效方法和初步的数据支持。

In order to provide technology support for quality“Gui-pu No.1”Vitis quinnquangularis Rehd winemaking,the quantitative method of 9 classic phenolic compounds was developed by HPLC,and the changes of their fermentation process were tracked.After wave length and gradient optimization,the final optimized analytical condition were fixed as follows:The column was Atlanis T3 column(4.6 mm×250 mm,5μm),flow rate was 1 mL/min,gradient elution was adopted,column temperature was 30℃,detection wavelength was 280,306,320,360 nm,respectively,and sample loading volume was 10μL.This method was proven to be a wide linear range,R2>0.989,as well as quantitative limits were from 0.056 to 0.987 mg/L,recovery rates of gradient 4 of mixed standards were from 92.37%to 103.45%,relative standard deviations were not more than 3.26%.The results showed as following:Only kaempferol was not detected in the initial fermentation broth.The changes module of different phenolic acid contents in the ferment broth of“Gui-pu No.1”during fermentation process at 22℃and 28℃were different.In contrast the declining trend of polydatin and chlorogenic acid during fermentation process,the changes of other phenolic compounds showed as a trend of increasing first and then decreasing.The variation trends of same compound at different fermentation temperature of 22℃and 28℃were basically the same,but the variation magnitudes were different.In the fermentation broths at 22℃and 28℃for 15 d,only the contents of cyandin-3-O-glucoside,kaempferol and ferulic acid were all higher than those in the initial fermentation broths.This study provided effective quality controlling means and preliminary data support for the quality production of phenolic compounds in Vitis quinnquangularis Rehd winemaking.