CN113425754A - 一种从百香果果皮中联合提取黄酮和果胶的方法 - Google Patents
一种从百香果果皮中联合提取黄酮和果胶的方法 Download PDFInfo
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Abstract
本发明公开了一种从百香果果皮中联合提取黄酮和果胶的方法，包括以下步骤：清洗，烘干，粉碎，得百香果果皮粉末；将百香果果皮粉末加入提取罐中，加入乙醇、增溶剂三乙醇胺和碳酸二甲酯，并用碱调节pH至8.0~8.5，超声波提取，过滤，分离滤液A和滤渣A；滤液A过柱、减压蒸馏，得百香果果皮总黄酮；取滤渣A，灭酶活，加入水，Tween‑80和纤维素酶，浸泡并超声波提取5~15min，过滤，分离滤液B和滤渣B；滤液B减压浓缩、脱色，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。通过本发明能实现从百香果果皮中联合提取黄酮和果胶，实现百香果果皮的综合利用。
Description
技术领域
本发明涉及提取工艺技术领域，尤其是一种从百香果果皮中联合提取黄酮和果胶的方法。
背景技术
百香果原产南美洲，是西番莲科西番莲属的一种多年生藤本植物，因其果汁散发出香蕉、菠萝、柠蒙、草莓、番桃、石榴等多种水果的浓郁香味而被誉为“百香果”，也是其英文名“Passionfruit”的译音，在国外还有“果汁之王”、“摇钱树”等美称。
百香果的果汁色、香、味、营养极佳，富含人体必需的17种氨基酸及多种维生素、微量元素等160多种有益成份，具有消除疲劳、提神醒酒、降脂降压、消炎祛斑、护肤养颜等神奇功效。
百香果在我国主要栽培于广西、广东、海南等华南省份及中国台湾地区，其中，广西是我国最大的百香果产区，百香果目前一般将其果肉用于生产果汁、果冻、果露、果酱等产品，而其果皮常常被当做废料直接丢弃，如此造成资源的浪费，还可能带来环境污染等相关问题。根据相关文献报道，百香果果皮中含有大量的生物活性物质，如多糖、果胶、黄酮。黄酮类化合物具有减除烦躁和缓解压力的作用；果胶是人体七大营养素中膳食纤维的主要成分，具有良好的抗腹泻、抗癌、治疗糖尿病和减肥等功效，而百香果的果皮中约含有3%的果胶（按照新鲜果皮质量计算），其果胶中的甲氧基含量是水果之冠，若能从百香果果皮中联合提取黄酮和果胶，将实现废弃物的回收再利用，同时能更好的满足医药、化妆品、食品领域的功能性需求。
发明内容
本发明公开了一种从百香果果皮中联合提取黄酮和果胶的方法，能实现从百香果果皮中联合提取黄酮和果胶，实现百香果果皮的综合利用。
为实现上述目的，本发明的技术方案为：
一种从百香果果皮中联合提取黄酮和果胶的方法，包括以下步骤：
S1.将百香果果皮清洗干净，35~45℃烘干，粉碎，得百香果果皮粉末；
S2.将百香果果皮粉末加入提取罐中，并按照固液比1：40~60g/mL，加入体积分数为75~85%的乙醇，同时加入增溶剂三乙醇胺和碳酸二甲酯，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:3~6:5~10，并用碱调节pH至8.0~8.5，超声波提取20~30min，温度为45~55℃，提取1~2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/8~1/10，调节pH至6.5~7.5，滤液过大孔树脂柱，用65~80%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4. 取滤渣A，加入沸水中处理5~10min，过滤，清洗，压干，按照固液比1:3~8 g/mL加入水，再以水的质量计，加入0.1~0.2wt%的Tween-80和0.1~0.3wt%的纤维素酶，浸泡20~30min，然后加入水调节固液比至1:12~18 g/mL，用酸调节溶液pH至1.5~2.0，超声波提取5~15min，加热灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5.滤液B减压浓缩、脱色，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
优选的，所述步骤S2中，超声波的功率为220~250W。
优选的，所述步骤S3中，大孔树脂柱为D101大孔树脂柱。
优选的，所述步骤S4中，超声波的功率为600~800W。
优选的，脱色的步骤具体为：在滤液B减压浓缩后，取所得的浓缩液，加入浓缩液质量1~3%的活性炭或硅藻土，搅拌脱色45~70min。
优选的，所述步骤S5中，减压浓缩时，浓缩至滤液B体积的1/6~1/10。
优选的，所述步骤S2中，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:3:8。
优选的，所述步骤S4中，以水的质量计，加入0.12wt%的Tween-80和0.2wt%的纤维素酶。
优选的，所述步骤S4中，调节pH的酸为酒石酸或柠檬酸。
以上所述的从百香果果皮中联合提取黄酮和果胶的方法，具有以下优点：
（1）本发明先在碱性条件下采用超声波法对总黄酮进行提取，通过碱性条件抑制果胶的溶出，同时采用三乙醇胺和碳酸二甲酯共同作用，通过有机溶剂和适宜的温度提高总黄酮的溶出率，减少总黄酮的氧化，且使果胶最大限度的保留在滤渣中。
（2）本发明在提取总黄酮之后，再加入Tween-80改变果皮细胞内外的渗透压，改变细胞的通透性，同时加以纤维素酶快速破坏细胞壁，在破坏细胞壁之后，协同酸性pH条件以及超声波提取，使果胶尽可能的游离出来，提高百香果果胶的提取率。
（3）采用本发明能同时提取黄酮和果胶，能使百香果果皮的利用价值最大化，同时更好的满足医药、化妆品、食品领域的功能性需求。
具体实施方式
以下结合具体实施例对本发明作进一步说明，但本发明的保护范围不限于以下实施例。
以下实施例采用的纤维素酶的酶活为2.0×105U/g。
总黄酮提取率的测定，采用“逆流法提取百香果果皮中总黄酮的工艺研究”（廖兰、吴俊良，广西科技大学[J]，2018,29(02)：91-96）中的方法。
果胶得率测定，采用“微波法提取百香果果胶的方法研究”（朱帝、陈采莹，绍兴文理学院化学化工学院[J]，2020,31(14)：29-30）中的方法。
百香果，购买于南宁市。
步骤S1中，均采用统一处理，45℃烘干粉碎，得百香果果皮粉末。
实施例1
一种从百香果果皮中联合提取黄酮和果胶的方法，包括以下步骤：
S1.将百香果果皮清洗干净，45℃烘干，粉碎，得百香果果皮粉末；
S2.将1kg百香果果皮粉末加入提取罐中，并按照固液比1：48g/mL，加入体积分数为80%的乙醇，同时加入增溶剂三乙醇胺和碳酸二甲酯，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:3:8，并用氢氧化钠调节pH至8.5，超声波提取30min，超声波的功率为230W，温度为52℃，提取2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/8，用盐酸调节pH至7.2，滤液过D101大孔树脂柱，用65%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理8min，过滤，清洗滤渣，压干，按照固液比1:4 g/mL加入水，再以水的质量计，加入0.12wt%的Tween-80和0.2wt%的纤维素酶，浸泡25min，然后加入水调节固液比至1:15 g/mL，用酒石酸调节溶液pH至1.8，超声波提取7min，加热90℃保温7min灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5.滤液B减压浓缩，浓缩至滤液B体积的1/8，得浓缩液，加入浓缩液质量3%的活性炭脱色，搅拌脱色60min，分离出活性炭后，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
经测试，总黄酮的提取率为2.75%，果胶得率为27.12%。
实施例2
一种从百香果果皮中联合提取黄酮和果胶的方法，包括以下步骤：
S1.将百香果果皮清洗干净，45℃烘干，粉碎，得百香果果皮粉末；
S2.将1kg百香果果皮粉末加入提取罐中，并按照固液比1：40g/mL，加入体积分数为75%的乙醇，同时加入增溶剂三乙醇胺和碳酸二甲酯，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:3:5，并用氢氧化钠调节pH至8.0，超声波提取30min，超声波的功率为250W，温度为50℃，提取2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/10，用盐酸调节pH至6.8，滤液过D101大孔树脂柱，用70%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理10min，过滤，清洗滤渣，压干，按照固液比1:5 g/mL加入水，再以水的质量计，加入0.1wt%的Tween-80和0.3wt%的纤维素酶，浸泡25min，用柠檬酸调节溶液pH至1.8，然后加入水调节液固比至1:12 g/mL，超声波提取10min，加热90℃保温10min灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5.滤液B减压浓缩，浓缩至滤液B体积的1/6，得浓缩液，加入浓缩液质量3%的硅藻土脱色，搅拌脱色50min，分离出硅藻土后，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
经测试，总黄酮的提取率为2.52%，果胶得率为23.31%。
实施例3
一种从百香果果皮中联合提取黄酮和果胶的方法，包括以下步骤：
S1.将百香果果皮清洗干净，45℃烘干，粉碎，得百香果果皮粉末；
S2.将1kg百香果果皮粉末加入提取罐中，并按照固液比1：60g/mL，加入体积分数为75%的乙醇，同时加入增溶剂三乙醇胺和碳酸二甲酯，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:6:5，并用氢氧化钠调节pH至8.5，超声波提取30min，超声波的功率为220W，温度为55℃，提取2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/10，用盐酸调节pH至7.5，滤液过D101大孔树脂柱，用70%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理10min，过滤，清洗滤渣，压干，按照固液比1:5g/mL加入水，再以水的质量计，加入0.2wt%的Tween-80和0.1wt%的纤维素酶，加入纤维素酶，浸泡25min，用酒石酸调节溶液pH至1.8，然后加入水调节液固比至1:18 g/mL，超声波提取5min，加热90℃保温10min灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5. 滤液B减压浓缩，浓缩至滤液B体积的1/10，得浓缩液，加入浓缩液质量3%的活性炭脱色，搅拌脱色70min，分离出活性炭后，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
经测试，总黄酮的提取率为2.81%，果胶得率为21.26%。
对比例1
一种从百香果果皮中联合提取黄酮和果胶的方法，包括以下步骤：
S1.将百香果果皮清洗干净，45℃烘干，粉碎，得百香果果皮粉末；
S2.将1kg百香果果皮粉末加入提取罐中，并按照固液比1：48g/mL，加入体积分数为75%的乙醇，超声波提取30min，超声波的功率为230W，温度为52℃，提取2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/8，滤液过D101大孔树脂柱，用65%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理8min，过滤，清洗滤渣，压干，按照固液比1:6 g/mL加入水，再以水的质量计，加入0.12wt%的Tween-80和0.2wt%的纤维素酶，浸泡25min，用酒石酸调节溶液pH至1.8，然后加入水调节液固比至1:15 g/mL，超声波提取25min，加热90℃保温10min灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5. 滤液B减压浓缩，浓缩至滤液B体积的1/8，得浓缩液，加入浓缩液质量3%的活性炭脱色，搅拌脱色60min，分离出活性炭后，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
经测试，总黄酮的提取率为2.11%，果胶得率为15.26%。
对比例2
S1.将百香果果皮清洗干净，45℃烘干，粉碎，得百香果果皮粉末；
S2.将1kg百香果果皮粉末加入提取罐中，并按照固液比1：48g/mL，加入体积分数为75%的乙醇，同时加入增溶剂三乙醇胺，乙醇和三乙醇胺的体积比为1000:11，并用氢氧化钠调节pH至8.5，超声波提取30min，超声波的功率为230W，温度为52℃，提取2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/8，用盐酸调节pH至7.2，滤液过D101大孔树脂柱，用65%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理8min，过滤，清洗滤渣，压干，按照固液比1:6 g/mL加入水，再以水的质量计，加入0.12wt%的Tween-80和0.2wt%的纤维素酶，浸泡25min，用酒石酸调节溶液pH至1.8，然后加入水调节液固比至1:15 g/mL，超声波提取25min，加热90℃保温10min灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5. 滤液B减压浓缩，浓缩至滤液B体积的1/8，得浓缩液，加入浓缩液质量3%的活性炭脱色，搅拌脱色60min，分离出活性炭后，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
经测试，总黄酮的提取率为2.19%，果胶得率为19.03%。
对比例3
S1.将百香果果皮清洗干净，45℃烘干，粉碎，得百香果果皮粉末；
S2.将1kg百香果果皮粉末加入提取罐中，并按照固液比1：48g/mL，加入体积分数为75%的乙醇，同时加入增溶剂碳酸二甲酯，乙醇和碳酸二甲酯的体积比为1000:11，并用氢氧化钠调节pH至8.0，超声波提取30min，超声波的功率为230W，温度为52℃，提取2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/8，用盐酸调节pH至7.2，滤液过D101大孔树脂柱，用65%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理8min，过滤，清洗滤渣，压干，按照固液比1:6 g/mL加入水，再以水的质量计，加入0.12wt%的Tween-80和0.2wt%的纤维素酶，浸泡25min，然后加入水调节液固比至1:15 g/mL，用酒石酸调节溶液pH至1.8，超声波提取25min，加热90℃保温10min灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5. 滤液B减压浓缩，浓缩至滤液B体积的1/8，得浓缩液，加入浓缩液质量3%的活性炭脱色，搅拌脱色60min，分离出活性炭后，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
经测试，总黄酮的提取率为2.26%，果胶得率为16.51%。
对比例4
S1.将百香果果皮清洗干净，45℃烘干，粉碎，得百香果果皮粉末；
S2.将1kg百香果果皮粉末加入提取罐中，并按照固液比1：48g/mL，加入体积分数为75%的乙醇，同时加入增溶剂三乙醇胺和碳酸二甲酯，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:3:8，并用氢氧化钠调节pH至8.5，超声波提取30min，超声波的功率为230W，温度为52℃，提取2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/8，用盐酸调节pH至7.2，滤液过D101大孔树脂柱，用65%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理8min，过滤，清洗滤渣，压干，按照固液比1:6 g/mL加入水，再以水的质量计，加入0.2wt%的纤维素酶，浸泡25min，然后加入水调节液固比至1:15g/mL，用酒石酸调节溶液pH至1.8，超声波提取25min，加热90℃保温10min灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5. 滤液B减压浓缩，浓缩至滤液B体积的1/8，得浓缩液，加入浓缩液质量3%的活性炭脱色，搅拌脱色60min，分离出活性炭后，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
经测试，总黄酮的提取率为2.72%，果胶得率为20.01%。
Claims (9)
1.一种从百香果果皮中联合提取黄酮和果胶的方法，其特征在于包括以下步骤：
S1.将百香果果皮清洗干净，35~45℃烘干，粉碎，得百香果果皮粉末；
S2.将百香果果皮粉末加入提取罐中，并按照固液比1：40~60g/mL，加入体积分数为75~85%的乙醇，同时加入增溶剂三乙醇胺和碳酸二甲酯，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:3~6:5~10，并用碱调节pH至8.0~8.5，超声波提取20~30min，温度为45~55℃，提取1~2次，过滤，分离滤液A和滤渣A；
S3.滤液A减压浓缩至原体积的1/8~1/10，调节pH至6.5~7.5，滤液过大孔树脂柱，用65~80%的乙醇洗脱，收集并合并洗脱液，洗脱液减压蒸馏，即获得百香果果皮总黄酮；
S4.取滤渣A，加入沸水中处理5~10min，过滤，清洗，压干，按照固液比1:3~8 g/mL加入水，再以水的质量计，加入0.1~0.2wt%的Tween-80和0.1~0.3wt%的纤维素酶，浸泡20~30min，然后加入水调节固液比至1:12~18 g/mL，用酸调节溶液pH至1.5~2.0，超声波提取5~15min，加热灭酶活，冷却后过滤，分离滤液B和滤渣B；
S5.滤液B减压浓缩、脱色，醇析，过滤后取沉淀物，沉淀物干燥，得果胶。
2.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S2中，超声波的功率为220~250W。
3.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S3中，大孔树脂柱为D101大孔树脂柱。
4.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S4中，超声波的功率为600~800W。
5.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S5中，脱色的步骤具体为：在滤液B减压浓缩后，取所得的浓缩液，加入浓缩液质量1~3%的活性炭或硅藻土，搅拌脱色45~70min。
6.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S5中，减压浓缩时，浓缩至滤液B体积的1/6~1/10。
7.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S2中，乙醇、三乙醇胺和碳酸二甲酯的体积比为1000:3:8。
8.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S4中，以水的质量计，加入0.12wt%的Tween-80和0.2wt%的纤维素酶。
9.根据权利要求1所述的从百香果果皮中联合提取黄酮和果胶的方法，其特征在于：
所述步骤S4中，调节pH的酸为酒石酸或柠檬酸。
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