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

作　　者：张芳芳 徐玲萍 朱欢智 ZHANG Fang-Fang;XU Ling-Ping;ZHU Huan-Zhi(Taizhou Food and Drug Inspection and Research Institute,Key Laboratory of Quality Safety and Quality Improvement of Special Agricultural Products in Taizhou City,Taizhou 318000,China)

机构地区：[1]台州市食品药品检验研究院,台州市特色农产品质量安全与品质提升重点实验室,台州318000

出　　处：《食品安全质量检测学报》2024年第23期310-317,共8页Journal of Food Safety and Quality

基　　金：台州市科技计划项目(22nyb04)。

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 C_(18)色谱柱(250 mm×4.6 mm,5μm)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5.0~200.0μg/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0.0561~0.4428μg/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。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 C_(18)column(250 mm×4.6 mm,5μm),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 5.0-200.0μg/mL,and the correlation coefficient(r)was greater than 0.999.The limit of detection of each compound was 0.0561-0.4428μg/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.

关 键 词：高效液相色谱法 发酵型杨梅酒 酚酸化合物 护色工艺 

分 类 号：TS262.7[轻工技术与工程—发酵工程] O657.72[轻工技术与工程—食品科学与工程]