酱油发酵基料酱油酮的提取及分析检测方法研究

Extraction and analysis of soy sauce ketone from soy sauce fermentation base

选用二氯甲烷、无水乙醇、无水乙醚为提取的有机溶剂,从5种酱油发酵基料中提取酱油酮后,用高效液相色谱法检测不同原料中酱油酮的含量。实验结果表明,高效液相色谱仪检测酱油酮的最佳液相条件为:甲醇∶水=30∶70;流速1 mL/min。从酱油发酵基料中提取酱油酮的最佳有机溶剂为二氯甲烷,其次是无水乙醇和乙醚。以萃取效果最佳的二氯甲烷为例,经过低温连续相变之后的基料,油中酱油酮的浓度对比原渣由11.190增加到91.653 mg/kg,说明原渣经过低温连续相变萃取后,酱油酮得到富集。而脱脂渣经过乙醇浓缩后,浓缩醇提物的酱油酮浓度对比醇提渣由5.134增加到27.959 mg/kg,说明经过乙醇浓缩后酱油酮进行了富集。

Dichloromethane,absolute ethanol,and anhydrous ether were selected as organic solvents for extraction.The content of the extracted soy sauce ketone from five kinds of soy sauce fermentation base was detected by high performance liquid chromatography(HPLC)after extracting soy sauce ketone from different raw materials.The results showed that the optimum conditions for the determination of ketone in soy sauce by HPLC were as follows:the ratio of methanol–water=30∶70 and a flow rate of 1 mL/min.The solvent dichloromethane was tested as the best organic solvent for extracting soy sauce ketone from soy sauce fermentation base,followed by ethanol and anhydrous ether.Taking dichloromethane with the best extraction effect as an example,after low-temperature continuous phase transition of the base material,the concentration of soy sauce ketone in the oil increased from 11.190 to 91.653 mg/kg compared to the original residue,indicating that soy sauce ketone was enriched after low-temperature continuous phase transition extraction of the original residue.After ethanol concentration of the defatted residue,the concentration of soy sauce ketone in the concentrated ethanol extract increased from 5.134 to 27.959 mg/kg compared to the ethanolextracted residue,indicating that soy sauce ketone was enriched after ethanol concentration.