高效液相色谱法同时测定发酵型杨梅酒中11种酚酸类化合物

Simultaneous determination of 11 kinds of phenolic acid compounds in fermented bayberry wine by high performance liquid chromatography

中文关键词:  高效液相色谱法  发酵型杨梅酒  酚酸化合物  不同护色工艺

英文关键词:high performance liquid chromatography  fermented bayberry wine  phenolic acid compounds  color protection technology

中文摘要:

      目的 建立高效液相色谱法同时测定发酵型杨梅酒中11种类酚酸化合物(没食子酸、原儿茶酸、4-羟基苯甲酸、绿原酸、龙胆酸、香草酸、咖啡酸、丁香酸、对香豆酸、阿魏酸和芥子酸)的分析方法。方法 试样经碱性水解液提取处理后水解为游离酚酸化合物, 采用SunFire C18色谱柱(250 mm×4.6 mm, 5 μm)分离, 甲醇-乙酸-水作为流动相梯度洗脱, 280 nm和320 nm波长下检测分析, 外标法定量。结果 11种酚酸化合物在5.0~200.0 μg/mL各自相应的范围内线性关系良好, 相关系数(r)均大于0.999, 各化合物的检出限为0.0561~0.4428 μg/mL, 3个不同浓度添加水平的加标回收率为91.61%~108.40%, 相对标准偏差(relative standard deviations, RSDs)为1.71%~4.23%。未添加辅色剂杨梅酒中11种酚酸类化合物均有检出, 没食子酸含量最高, 占11种酚酸化合物总量的58%; 原儿茶酸次之, 约占11种酚酸化合物总量的35%; 对添加抗坏血酸、单宁、苯甲酸、乙二胺四乙酸、二氧化硫5种不同含量辅色剂开展护色工艺研究的杨梅酒进行测定, 发现添加0.15 mg/L单宁或添加0.05 mg/L抗坏血酸的杨梅酒对酚酸化合物含量影响最小。结论 该方法准确度和精密度较高, 适用于发酵型杨梅酒中酚酸类化合物的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 11 kinds of phenolic acid compounds (gallic acid, protocatechuic acid, 4-hydroxybenzoic acid, chlorogenic acid, gentian acid, vanillic acid, caffeic acid, syringic acid, p-coumaric acid, ferulic acid and erucic acid) in fermented bayberry wine by high performance liquid chromatography. Methods The samples were extracted by alkaline hydrolysate and hydrolyzed to free phenolic acid compounds. The samples were separated by SunFire C18 column (250 mm×4.6 mm, 5 μm), eluted by methanol-acetic acid-water as mobile phase gradient, detected at 280 nm and 320 nm, and quantified by external standard method. Results The linear relationship of 11 kinds of phenolic acid compounds was good in the corresponding range of 5.0–200.0 μg/mL, and the correlation coefficient (r) was greater than 0.999. The limit of detection of each compound was 0.0561–0.4428 μg/mL, and 3 kinds of different concentrations were added to the mark. The yield was 91.61%–108.40%, and the relative standard deviations (RSDs) were 1.71%–4.23%. All 11 kinds of phenolic acids were detected in bayberry wine without additive, the content of gallic acid was the highest, accounting for 58% of the total 11 kinds of phenolic acids. Protocatechuic acid was the second, accounting for about 35% of the total 11 kinds of phenolic acid compounds. Determination of color protection technology for bayberry wine with 5 kinds of different content auxiliary colorants including ascorbic acid, tannin, benzoic acid, ethylenediaminetetraacetic acid, and sulfur dioxide added, it was found that adding 0.15 mg/L tannin or 0.05 mg/L ascorbic acid in bayberry wine had the least effect on phenolic acid compound content. Conclusion The method has high accuracy and precision, and is suitable for the determination of phenolic acids in fermented bayberry wine.