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[摘要]
以液压核桃粕为原料,通过单因素试验和响应面设计优化核桃粕中多酚微波-超声分步共辅助提取工艺,采用超高效液相色谱-四级杆-飞行时间-质谱联用仪分析鉴定多酚化合物,通过DPPH、ABTS、羟自由基清除实验评估抗氧化活性,并反添加到核桃油中验证对油脂氧化稳定性的影响。结果表明料液比与乙醇体积分数对核桃粕中多酚提取量具有显著性影响(P<0.05),最佳提取工艺为:料液比1:57.33 g/mL,乙醇体积分数69.13%,超声功率100 W,微波功率109.92 W,核桃粕中多酚提取量为40.59 mg GAE/g。鉴定出核桃粕多酚化合物24种,其中含量较高的多酚质量溶度为3,4-二羟基苯乙酸(8233.93 μg/g)、山奈酚-3-O芸香糖苷(4504.20 μg/g)、鞣花酸(1882.50 μg/g)等。核桃粕多酚在质量浓度为0.80 mg/mL时具有较好的DPPH和ABTS自由基清除效果(95%以上),羟自由基清除率维持在60%-70%;核桃粕多酚质量分数为0.08%时,可以将核桃油的氧化稳定性提高30%以上。核桃粕多酚作为天然抗氧化剂,进一步分离纯化后在食品行业具有很高的应用价值。
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[Abstract]
Using hydraulic walnut meal as the raw material, the polyphenols in walnut meal were extracted using a microwave-ultrasound co-assisted extraction process optimized by single-factor experiments and response surface design. Ultra-high-performance liquid chromatography-tandem mass spectrometry-time of flight mass spectrometry (UPLC Q-TOF/MS) was employed to analyze and identify polyphenolic compounds. The antioxidant activity was evaluated through DPPH, ABTS, and hydroxyl radical scavenging assays, and the extracts were added back to walnut oil to verify their impact on the oxidative stability. The results indicated that the solid-liquid ratio and the volume fraction of ethanol significantly affected the extraction of polyphenols from walnut meal (P<0.05). The optimal extraction conditions were the solid-liquid ratio of 1:57.33 g/mL, the ethanol volume fraction of 69.13%, ultrasonic power of 100 W, and microwave power of 109.92 W, the polyphenol extraction yield was of 40.59 mg GAE/g from walnut meal. A total of 24 polyphenolic compounds were identified, with higher contents of 3,4-dihydroxybenzoic acid (8233.93 μg/g), kaempferol-3-O-rutinoside (4504.20 μg/g), and ellagic acid (1882.50 μg/g). Walnut meal polyphenols exhibited good DPPH and ABTS radical scavenging effects (over 95%) at a mass concentration of 0.80 mg/mL and maintained a hydroxyl radical scavenging rate of 60%-70%. At a mass concentration of 0.08%, walnut meal polyphenols could increase the oxidative stability of walnut oil by more than 30%. As natural antioxidants, walnut meal polyphenols had high application value in the food industry after further separation and purification.
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