CN108157965A - 一种三七花提取物的制备方法及应用 - Google Patents
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Abstract
本发明公开了一种三七花提取物的制备方法，该方法利用微波灭菌灭酶干燥处理、生物酶解降解农残，然后经超声提取和热回流提取得三七花粗提取物，粗提取物进一步使用小孔径树脂柱吸附农残、纳滤处理脱农残，冷冻干燥获得三七花提取物，本发明方法简单易行，能在高效去除农残的同时，保留三七花中皂苷、多酚、黄酮、多糖等有效成分，本发明方法制得固体速溶茶饮冲泡后具有鲜三七花的特有芬芳、微苦，回味，产品无农残、绿色、健康。
Description
技术领域
本发明涉及一种三七花提取物的制备方法及应用。
背景技术
三七花为五加科人参属植物三七（Panax pseudoginseng）花序的干燥品，三七花，质脆易碎，气微，味甘微苦，其含有人参多种皂苷、黄酮，具有平清热肝、降血脂、降血压、抗癌、提高心肌供氧能力、增强机体免疫等功能；三七花总皂甙对中枢神经系统呈抑制作用，表现为镇静、安神功效，三七花黄酮具有抗炎、改善微循环，降压作用；用于高血压，头昏、目眩、耳鸣，急性咽喉炎的治疗；传统服用方法多为泡水喝。
三七花苞含甙和黄酮、多酚、多糖类物质，皂苷中含有人参二醇（panaxadiol)，Rb1、Rb2、Rb3、Rc、Rd、F2等，含量大于15%，黄酮含量大于10%，多酚，多糖含量也较高。
三七种植面积不断扩大，在云南已经达到几十万亩，三七3年采收，三七在种植过程中病虫害较高，农户大量使用各种农药和禁用农药，民间有“三七无农药不活，靠药养三七”的说法，平均每周打农药不低于2次，三七花在花期农药喷灌过程中，相比起埋在土里的三七根由于直接接触农药喷淋，农药残留更严重，给用三七花药安全带来极大隐患。
三七花中农残超标较为严重，由于花期较短，基本在花期使用了什么农药，什么农药就超标，短暂花期，农药无法短期降解，农残超标项目较多，多为有机磷，有机氯。除虫菊脂类，例如对硫磷、马拉硫磷、甲基硫菌灵、腐霉利、五氯硝基苯经常检测到超标严重，其中一些农残超标超过100倍限度。
研究表明，农药残留对人体具有致癌、新生胎儿畸形和基因突变等作用，有机氯农残半衰期较长，在人体中代谢较慢，蓄积到一定量对人体危害较大。DDT能干扰人体内激素的平衡，影响男性生育力。有机磷和氨基甲酸酯类农药可抑制胆碱酯酶活性，破坏神经系统的正常功能；广泛使用的农药具有明显的致癌性；
三七根去农残使用水高压冲洗，短暂浸泡具有去除三七根中90%农残重金属的效果，并对有效成分损失较低，不超过0.5%。养生专家也建议三七花冲泡法为先用开水冲泡一次，倒掉再泡有去除农残的功效。冲泡洗涤法确实可去除大部分三七根农残，和部分三七花农残，然三七花质地疏松，有效成分基本均为水溶性成分，一次冲泡水损失5%的人参二醇皂苷，极大降低冲泡后的三七花有效物质含量。
常规方法水提不经去农残处理所得三七花提取物，完整保留了三七花全成分，然提取物中农药含量也急剧提升，超过三七花中几倍。利用现代生物技术，植物化学技术精制提取所得三七花皂苷，去除了农残，三花中二醇皂苷含量较高，药效更为明显，用药亦较为安全，然大部分三七花黄酮，花青素、多糖的损失大大降低了三七花抗炎，降压，改善微循环功效。
发明内容
本发明目的在于提供一种能高效去除农残的三七花提取物的制备方法，该方法利用现代生物技术制备所得三七花提取物，在去除农残的同时，保留了三七花特有芬芳、口感苦甘，回味，为有效成分全成分提取物；提取过程中集成了生物酶解农残技术、超声提取降解农残技术、小孔径树脂脱农残技术、纳滤脱盐脱农残技术等，有效去除了三七花中农残，产品绿色安全。
本发明方法按如下步骤进行：
（1）取新鲜三七花去花梗，在微波条件下处理10-15min后取出；
（2）将微波处理后的三七花置于质量浓度0.5-1.5%的磷脂酶溶液中浸泡3-5min，然后除去水分至没有液体滴出；
（3）将三七花置于微波条件下真空干燥至含水量小于3%；
（4）在干燥的三七花中加入其质量10-12倍的纯水，浸泡2-3h，然后于55-65℃下超声提取1-2h，三足离心机离心，得三七花超声提取液，有效成分提取率大于80%，该低温超声提降解农残并保留三七花特有香味；
（5）在超声提取后的药渣中再加入药渣质量5-6倍的纯水，于提取罐中在85-95℃下热回流提取2-3h，离心去除药渣，收集离心液；提取剩余三七花药渣中残余有效成分；
（6）合并三七花超声提取液和步骤（5）离心液，过小孔径树脂柱脱农残，上柱流速为2-3倍柱体积/每小时，收集流出液，流出液为三七花全成分提取物；由于树脂孔径较小不吸附三七皂苷和黄酮等物质，树脂吸附物为小分子农残；
（7）将流出液用纳滤膜进行浓缩，同时进行纳滤脱盐脱农残，收集膜截留液，截留液为三七花提取物，弃流出液，流出液为水液、农残、农残降解物、盐类、色素等杂质；
（8）膜截留液在20000-25000r/min下高速离心，收集澄清离心液冷冻干燥后，即得三七花提取物。
所述步骤（1）中微波功率为1800-2500w。
所述步骤（3）中微波功率为500-700w。
所述步骤（4）中超声提取功率为10-15MHz。
所述小孔径树脂型号为LX-220，树脂孔径为20-30A。
所述小孔径树脂柱是用体积浓度95%的乙醇浸泡小孔径树脂8h以上，水洗至无醇后，取2-3倍生药量的树脂湿法装柱而成。
所述纳滤膜的截流分子量为200-250。
本发明另一目的是将上述三七花提取物的制备方法制得三七花提取物应用在制备三七花速溶茶中。
本发明方法的优点和技术效果：
1、微波达到一定频率可以降解部分农残；
2、磷脂酶可以水解磷脂键达到农残降解的目的，特别针对有机磷农残；
3、超声提取时候超声波可以降解农残，改变或破坏农残结构，低温提取同时保留了三七花的香味和口感；加热热回流提取，提取药渣中残余有效物质同时热降解药渣中热敏性农残，达到进一步热裂解农残的作用；
4、小孔径树脂吸附200分子以下的农残，对芳香类农残去除效果非常好；
5、纳滤膜过滤可以滤过掉农残和农残降解产物，植物中大部分农残分子量都小于200，膜分离使得残余农残和农残降解产物通过过滤方式去除。
本发明方法简单易行，能在高效去除农残的同时，保留三七花中皂苷、多酚、黄酮、多糖等有效成分，本发明方法制得固体速溶茶饮冲泡后具有鲜三七花的特有芬芳、微苦，回味，产品无农残、绿色、健康；该三七花提取物具有抗炎，清除氧自由基，促进学习记忆，改善睡眠，抗衰老，强壮滋补功效。
具体实施方式
下面通过实施例对本发明作进一步详细说明，但本发明保护范围不局限于所述内容。
实施例1：本三七花提取物的制备方法的具体操作如下：
（1）取新鲜三七花去花梗得花蕾，在微波功率2000w下微波处理12min后取出；
（2）将微波处理后的三七花置于质量浓度0.5%的磷脂酶溶液中浸泡5min，然后取出筛网晾晒除去水分至没有液体滴出；
（3）将三七花置于微波功率为500w下真空干燥至含水量为2%；
（4）在干燥的三七花中加入其质量10倍的纯水，浸泡2h，然后于55℃下超声（超声提取功率为10MHz）提取2h，三足离心机离心，得三七花超声提取液；
（5）在超声提取后的药渣中再加入药渣质量5倍的纯水，于提取罐中在85℃下热回流提取3h，三足离心机离心去除药渣，收集离心液；
（6）合并三七花超声提取液和步骤（5）离心液，过小孔径树脂（型号为LX-220，树脂孔径为20A，用体积浓度95%乙醇浸泡小孔径树脂9h，水洗至无醇后，取2倍生药量的树脂湿法装柱）柱脱农残，上柱流速为2倍柱体积/每小时，收集流出液，流出液为三七花全成分提取物；
（7）将流出液用纳滤膜（截留分子量200）进行浓缩，收集膜截留液，截留液为三七花提取物，弃流出液；
（8）膜截留液在20000r/min下高速离心，收集澄清离心液冷冻干燥后，即得三七花提取物，该提取物Rb3含量15.12%，有机磷农残小于5ppm，有机氯农残小于5ppm；
将上述三七花提取物用于制备三七花速溶茶，经粉碎，分装每袋1克，无需任何辅料添加，所制得的产品口感苦甘，回味，具有三七花特有的香味。
实施例2：本三七花提取物的制备方法的具体操作如下：
（1）取新鲜三七花去花梗得花蕾，在微波功率2500w下微波处理10min后取出；
（2）将微波处理后的三七花置于质量浓度1%的磷脂酶溶液中浸泡4min，然后取出筛网晾晒除去水分至没有液体滴出；
（3）将三七花置于微波功率为600w下真空干燥至含水量为1%；
（4）在干燥的三七花中加入其质量11倍的纯水，浸泡3h，然后于60℃下超声（超声提取功率为12MHz）提取1.5h，三足离心机离心，得三七花超声提取液；
（5）在超声提取后的药渣中再加入药渣质量6倍的纯水，于提取罐中在90℃下热回流提取2.5h，三足离心机离心去除药渣，收集离心液；
（6）合并三七花超声提取液和步骤（5）离心液，过小孔径树脂（型号为LX-220，树脂孔径为30A，用体积浓度95%乙醇浸泡小孔径树脂9h，水洗至无醇后，取3倍生药量的树脂湿法装柱）柱脱农残，上柱流速为3倍柱体积/每小时，收集流出液，流出液为三七花全成分提取物；
（7）将流出液用纳滤膜（截留分子量250）进行浓缩，收集膜截留液，截留液为三七花提取物，弃流出液；
（8）截留液在22000r/min下高速离心，收集澄清离心液冷冻干燥后，即得三七花提取物，该提取物Rb3含量17.10%，有机磷农残小于5ppm，有机氯农残小于5ppm；
将上述三七花提取物用于制备三七花速溶茶，经粉碎，分装每袋1克，无需任何辅料添加，所制得的产品口感苦甘，回味，具有三七花特有的香味。
实施例3：本三七花提取物的制备方法的具体操作如下：
（1）取新鲜三七花去花梗得花蕾，在微波功率1900w下微波处理15min后取出；
（2）将微波处理后的三七花置于质量浓度1.5%的磷脂酶溶液中浸泡3min，然后取出筛网晾晒除去水分至没有液体滴出；
（3）将三七花置于微波功率为700w下真空干燥至含水量为2%；
（4）在干燥的三七花中加入其质量12倍的纯水，浸泡2.5h，然后于65℃下超声（超声提取功率为15MHz）提取1h，三足离心机离心，得三七花超声提取液；
（5）在超声提取后的药渣中再加入药渣质量6倍的纯水，于提取罐中在95℃下热回流提取2h，三足离心机离心去除药渣，收集离心液；
（6）合并三七花超声提取液和步骤（5）离心液，过小孔径树脂（型号为LX-220，树脂孔径为30A，用体积浓度95%乙醇浸泡小孔径树脂,10h，水洗至无醇后，取2倍生药量的树脂湿法装柱）柱脱农残，上柱流速为2.5倍柱体积/每小时，收集流出液，流出液为三七花全成分提取物；
（7）将流出液用纳滤膜（截留分子量200）进行浓缩，收集膜截留液，截留液为三七花提取物，弃流出液；
（8）截留液在25000r/min下高速离心，收集澄清离心液冷冻干燥后，即得三七花提取物该提取物Rb3含量14.33%，有机磷农残小于5ppm，有机氯农残小于5ppm；
将上述三七花提取物用于制备三七花速溶茶，经粉碎，分装每袋1克，无需任何辅料添加，所制得的产品口感苦甘，回味，具有三七花特有的香味。
Claims (8)
1.一种三七花提取物的制备方法，其特征在于，按如下步骤进行：
（1）取新鲜三七花去花梗，在微波条件下处理10-15min后取出；
（2）将微波处理后的三七花置于质量浓度0.5-1.5%的磷脂酶溶液中浸泡3-5min，然后除去水分至没有液体滴出；
（3）将三七花置于微波条件下真空干燥至含水量小于3%；
（4）在干燥的三七花中加入其质量10-12倍的纯水，浸泡2-3h，然后于55-65℃下超声提取1-2h，三足离心机离心，得三七花超声提取液；
（5）在超声提取后的药渣中再加入药渣质量5-6倍的纯水，于提取罐中在85-95℃下热回流提取2-3h，离心去除药渣，收集离心液；
（6）合并三七花超声提取液和步骤（5）离心液，过小孔径树脂柱脱农残，上柱流速为2-3倍柱体积/每小时，收集流出液，流出液为三七花全成分提取物；
（7）将流出液用纳滤膜进行浓缩，收集膜截留液，截留液为三七花提取物，弃流出液；
（8）膜截留液在20000-25000r/min下高速离心，收集澄清离心液冷冻干燥后，即得三七花提取物。
2.根据权利要求1所述的三七花提取物的制备方法，其特征在于：步骤（1）中微波功率为1800-2500w。
3.根据权利要求1所述的三七花提取物的制备方法，其特征在于：步骤（3）中微波功率为500-700w。
4.根据权利要求1所述的三七花提取物的制备方法，其特征在于：步骤（4）中超声提取功率为10-15MHz。
5.根据权利要求1所述的三七花提取物的制备方法，其特征在于：小孔径树脂型号为LX-220，树脂孔径为20-30A。
6.根据权利要求1所述的三七花提取物的制备方法，其特征在于：小孔径树脂柱是用体积浓度95%乙醇浸泡小孔径树脂8h以上，水洗至无醇后，取2-3倍生药量的树脂湿法装柱而成。
7.根据权利要求1所述的三七花提取物的制备方法，其特征在于：纳滤膜的截流分子量为200-250。
8.权利要求1所述的三七花提取物的制备方法制得三七花提取物在制备三七花速溶茶中的应用。
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