贡柑皮多甲氧基黄酮的提取优化及其油脂抗氧化稳定性研究

Study on the optimum extraction of polymethoxy flavonoids from Tribute citrus peels and their antioxidative stability in oil

中文关键词:  贡柑皮多甲氧基黄酮  响应面法  结构鉴定  抗氧化活性

英文关键词:polymethoxy flavonoids from Tribute citrus peels  response surface methodology  structural identification  antioxidant activity

中文摘要:

      目的 优化德庆贡柑皮多甲氧基黄酮的提取, 并探究其对油脂抗氧化稳定性的影响。方法 在单因素实验基础上, 根据Box-Benhnken的中心组合设计实验, 采用响应面法对贡柑皮中多甲氧基黄酮(polymethoxy flavonoids, PMFs)的提取工艺进行优化; 采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)分析贡柑皮中PMFs组分。结果 提取的最佳工艺参数为: 料液比1:3.23 (g:mL)、乙醇浓度87%、超声提取时间46 min, 提取率为6.87%; 贡柑皮中含有6种PMFs, 分别为橘皮素、川陈皮素、5-羟基-2’,4’,7,8-四甲氧基黄酮、黄芩黄酮II、栀子黄素B、5-去甲基川陈皮素, 相对质量浓度分别为10494.1、8428.4、826.3、678.4、141.3、12.0 μg/mL; 贡柑皮PMFs提取物对1,1-二苯基-2-三硝基苯肼(1,1-diphenyl-2-picrylhydrazyl, DPPH)和2,2’-联氮-二(3-乙基-苯并噻唑啉-6-磺酸)二铵盐[2,2’-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) ammonium salt, ABTS]+自由基具有清除作用, 当提取物质量浓度达到2.00 mg/mL时, 对DPPH自由基清除率为83.44%, 对ABTS+自由基清除率为77.56%; 贡柑皮PMFs提取物对油炸油饼中的油脂氧化具有一定的抑制作用, 在油炸时间5 h内, 添加1.00%贡柑皮PMFs提取物的样品显著降低了油脂的过氧化值和酸价, 而添加0.50%贡柑皮PMFs提取物的样品茴香胺值显著降低。结论 优化后的PMFs提取率为6.87%, 贡柑皮种含有6种PMFs, 对自由基有清除作用且对油脂氧化有抑制作用。

英文摘要:

      Objective To explore the extraction optimization of polymethoxy flavonoids from Tribute citrus peels and the effect on antioxidant stability in oil. Methods On the basis of single-factor experiments, the extraction of polymethoxy flavonoids (PMFs) from Tribute citrus peelsl was optimized using the Box-Behnken central composite design experiment and the response surface methodology. High performance liquid chromatography- tandem mass spectrometry (HPLC-MS/MS) was employed to analyze the PMFs components in Tribute citrus peels. Results The optimal extraction parameters were determined to be a solid-liquid ratio of 1:3.23 (g:mL), an ethanol concentration of 87%, an ultrasonic extraction time of 46 minutes, and an extraction rate of 6.87%; Tribute citrus peels contained 6 types of PMFs: Tangeritin, nobiletin, 5-hydroxy-2’,4’,7,8-tetramethoxyflavone, 5,2’-dihydroxy- 6,7,8,6’-tetramethoxy flavone, gardenin B and 5-demethylnobiletin, with a relative concentration of 10494.1, 8428.4, 826.3, 678.4, 141.3, 12.0 μg/mL; Tribute citrus peel PMFs had a certain scavenging ability for DPPH and ABTS+ radicals. When the mass concentration of PMFs reached 2.00 mg/mL, the scavenging rate for 1,1-diphenyl-2-picrylhydrazyl (DPPH) radicals was 83.44%, and the scavenging rate for 2,2’-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) ammonium salt (ABTS)+ radicals was 77.56%; the extract of PMFs from Tribute citrus peel had a certain inhibitory effect on the oxidation of oil in the fried Youbing. Within 5 hours of frying, the sample added 1.00% of the extract of PMFs from Tribute citrus peel significantly reduced the peroxide value and acid value of oil, while the sample added 0.50% of the extract of PMFs from Tribute citrus peel significantly reduced the anisidine value. Conclusion The optimized extraction yield of PMFs is 6.87%, and there are 6 types of PMFs in Tribute citrus peel, which have a scavenging effect on free radicals and an inhibitory effect on oil oxidation.