CN100556417C - Microwave Extraction Method of Total Flavonoids of Phytophthora - Google Patents
Microwave Extraction Method of Total Flavonoids of Phytophthora Download PDFInfo
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- 229930003935 flavonoid Natural products 0.000 title claims abstract description 20
- 150000002215 flavonoids Chemical class 0.000 title claims abstract description 20
- 235000017173 flavonoids Nutrition 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000000874 microwave-assisted extraction Methods 0.000 title claims abstract description 6
- 241000233614 Phytophthora Species 0.000 title abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 244000025254 Cannabis sativa Species 0.000 claims abstract description 12
- 235000014653 Carica parviflora Nutrition 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000469 ethanolic extract Substances 0.000 claims abstract description 4
- 239000005457 ice water Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 244000132059 Carica parviflora Species 0.000 claims abstract 3
- 241000196324 Embryophyta Species 0.000 claims description 2
- 238000010828 elution Methods 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 23
- 239000004480 active ingredient Substances 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
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- 241000243321 Cnidaria Species 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 238000000944 Soxhlet extraction Methods 0.000 description 3
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- 241000208829 Sambucus Species 0.000 description 1
- 235000018735 Sambucus canadensis Nutrition 0.000 description 1
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- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N benzo-alpha-pyrone Natural products C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 235000007123 blue elder Nutrition 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 150000004775 coumarins Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
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- 235000007124 elderberry Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
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- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
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- 230000001225 therapeutic effect Effects 0.000 description 1
- 241000712461 unidentified influenza virus Species 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
本发明公开了一种中药的提取方法，即草珊瑚总黄酮的微波浸提方法。其步骤为：取草珊瑚全草干燥并粉碎至60目，以固液比1∶40加入60%乙醇浸泡30分钟后，控制微波功率为900W，照射30秒，取出后冰水冷却，再照射30秒，同法操作重复3次。乙醇浸提液经减压浓缩后，过X-5型大孔吸附树脂，水洗后用70%乙醇洗脱，洗脱液减压浓缩干燥得草珊瑚总黄酮产品。本发明步骤简单、操作简便。以乙醇水溶液作为溶剂，无污染、无毒害，采用微波加热促进有效成分的提取，结合大孔吸附树脂进行分离，耗时短，提取效率高，产品的纯度较传统方法有明显的提高。The invention discloses a method for extracting traditional Chinese medicines, that is, a microwave extraction method for total flavonoids of Phytophthora flavonoids. The steps are as follows: take the whole coral coral grass, dry it and crush it to 60 mesh, add 60% ethanol to soak for 30 minutes at a solid-to-liquid ratio of 1:40, control the microwave power to 900W, irradiate for 30 seconds, take it out, cool it in ice water, and irradiate again For 30 seconds, repeat the same operation 3 times. The ethanol extract was concentrated under reduced pressure, passed through X-5 type macroporous adsorption resin, washed with water and eluted with 70% ethanol, and the eluate was concentrated and dried under reduced pressure to obtain the total flavonoids product of Grass coral. The invention has simple steps and convenient operation. Using ethanol aqueous solution as a solvent, it is non-polluting and non-toxic. Microwave heating is used to promote the extraction of active ingredients. Combining with macroporous adsorption resin for separation, the time-consuming is short, the extraction efficiency is high, and the purity of the product is significantly improved compared with traditional methods.
Description
技术领域 technical field
本发明涉及一种中药的提取方法，特别是草珊瑚总黄酮的微波浸提方法。The invention relates to a method for extracting traditional Chinese medicines, in particular to a microwave extraction method for total flavonoids of Phytophthora flavonoids.
背景技术 Background technique
草珊瑚又称肿节风、九节花、接骨莲，属金栗兰科半灌木植物，药性温、味苦辛。现代医学研究表明，草珊瑚具有抗菌消炎，抑制多种人、畜病原菌及流感病毒，抗肿瘤，促进骨折愈合，镇痛，安全无毒等多种活性，对多种人、畜疾病均有较好的治疗效果。草珊瑚全草含黄酮、香豆素、内酯、挥发油、有机酸及酚类、鞣质等物质，其中黄酮类物质为其主要有效成分。总黄酮传统的提取方法有水煎煮法、乙醇回流提取、索氏提取、渗漉法等，这些方法均存在提取时间长、提取效率低等问题。近些年又有新方法出现，如超声波提取、酶法提取等。超声波提取方法具有省时、节能、环保、提取效率高等优点，但提取效果易受仪器等因素的影响，如提取介质、放置位置、提取瓶壁厚薄、被超声物粒度等。酶法条件温和、提取的收率较高，但时间较长，提取的效率不高。微波提取方法是利用微波能短时间内使物质内部温度升高，促进目标物质的溶解，从而达到提取分离的目的。微波具有穿透力强、选择性高、加热效率高等特点，可以大大加快反应速度、缩短反应时间、提高目标物收率。到目前为止，尚未见有草珊瑚总黄酮的微波提取方法报道。Grass coral, also known as swollen knot wind, nine-section flower, and elderberry, is a semi-shrub plant of Chestnut orchidaceae, with warm medicinal properties and bitter and pungent taste. Modern medical research shows that grass coral has antibacterial and anti-inflammatory properties, inhibits a variety of human and animal pathogenic bacteria and influenza viruses, resists tumors, promotes fracture healing, analgesia, is safe and non-toxic, and has many activities. good therapeutic effect. Grass coral whole grass contains flavonoids, coumarins, lactones, volatile oils, organic acids, phenols, tannins and other substances, among which flavonoids are the main active ingredients. The traditional extraction methods of total flavonoids include water decoction, ethanol reflux extraction, Soxhlet extraction, percolation, etc. These methods all have problems such as long extraction time and low extraction efficiency. In recent years, new methods have emerged, such as ultrasonic extraction and enzymatic extraction. The ultrasonic extraction method has the advantages of time saving, energy saving, environmental protection, and high extraction efficiency, but the extraction effect is easily affected by factors such as the instrument, such as the extraction medium, the placement location, the thickness of the extraction bottle wall, and the particle size of the ultrasonic object. The enzymatic method has mild conditions and high extraction yield, but the time is long and the extraction efficiency is not high. The microwave extraction method uses microwave energy to increase the internal temperature of the substance in a short period of time to promote the dissolution of the target substance, thereby achieving the purpose of extraction and separation. Microwave has the characteristics of strong penetrating power, high selectivity, and high heating efficiency, which can greatly speed up the reaction speed, shorten the reaction time, and increase the yield of the target substance. So far, there has been no report on the microwave extraction method of total flavonoids from Coral praecox.
发明内容 Contents of the invention
本发明的目的在于提供一种低能高效的草珊瑚总黄酮的提取方法，它可以大大缩短提取时间、有效提高草珊瑚总黄酮的提取率。The object of the present invention is to provide a low-energy and high-efficiency extraction method of the total flavonoids of Coralia flavonoids, which can greatly shorten the extraction time and effectively improve the extraction rate of the total flavonoids of Corals frondosa.
本发明的技术方案如下：取草珊瑚全草干燥并粉碎至60目，以固液比1∶40加入60％乙醇浸泡30分钟后，控制微波功率为900W，照射30秒，取出后冰水冷却，再照射30秒，同法操作重复3次。乙醇浸提液经减压浓缩后，过X-5型大孔吸附树脂，水洗后用70％乙醇洗脱，洗脱液减压浓缩干燥得草珊瑚总黄酮产品。The technical scheme of the present invention is as follows: take the whole coral grass and dry it and crush it to 60 meshes, add 60% ethanol to soak for 30 minutes with a solid-to-liquid ratio of 1:40, control the microwave power to 900W, irradiate for 30 seconds, take it out and cool it in ice water , and then irradiate for 30 seconds, and repeat the same operation 3 times. The ethanol extract was concentrated under reduced pressure, passed through X-5 macroporous adsorption resin, washed with water, and eluted with 70% ethanol, and the eluate was concentrated and dried under reduced pressure to obtain the total flavonoids product of Grass coral.
本发明步骤简单、操作简便。以乙醇水溶液作为溶剂，无污染、无毒害，采用微波加热促进有效成分的提取，结合大孔吸附树脂进行分离，耗时短，提取效率高，产品的纯度较传统方法有明显的提高。The invention has simple steps and convenient operation. Using ethanol aqueous solution as a solvent, it is non-polluting and non-toxic. Microwave heating is used to promote the extraction of active ingredients. Combining with macroporous adsorption resin for separation, the time-consuming is short, the extraction efficiency is high, and the purity of the product is significantly improved compared with traditional methods.
具体实施方式 Detailed ways
实施例Example
取草珊瑚全草干燥并粉碎至60目，称取10g，加入60％乙醇400ml浸泡30分钟后，控制微波功率为900W，照射30秒，取出后冰水冷却，再照射30秒，同法操作重复3次。乙醇浸提液经减压浓缩回收乙醇，得浸提液。浸提液过X-5型大孔吸附树脂，先用蒸馏水洗，然后用70％乙醇洗脱，洗脱液减压浓缩干燥得草珊瑚总黄酮产品。以芦丁为标准对照，采用Al3+显色分光光度法测定总黄酮含量。提取物得率为7.12％，固形物中总黄酮含量为74.22％。Take the whole coral grass, dry it and crush it to 60 mesh, weigh 10g, add 400ml of 60% ethanol to soak for 30 minutes, control the microwave power to 900W, irradiate for 30 seconds, take it out and cool it in ice water, and then irradiate for 30 seconds, and operate in the same way Repeat 3 times. The ethanol extract is concentrated under reduced pressure to recover ethanol to obtain the extract. The extract is passed through the X-5 type macroporous adsorption resin, washed with distilled water, and then eluted with 70% ethanol, and the eluate is concentrated and dried under reduced pressure to obtain the total flavonoids product of Grass coral. With rutin as the standard control, the content of total flavonoids was determined by Al 3+ chromogenic spectrophotometry. The yield of the extract is 7.12%, and the total flavonoid content in the solid is 74.22%.
比较例1：工艺过程与实施例基本相同。不同之处是采用回流提取，不经微波处理，回流时间3小时。以下步骤同实施例。Comparative example 1: technological process is basically the same as embodiment. The difference is that reflux extraction is used without microwave treatment, and the reflux time is 3 hours. The following steps are the same as the examples.
比较例2：工艺过程与实施例基本相同。不同之处是采用索氏提取，不采用回流提取，不经微波处理，提取时间3小时。以下步骤同实施例。Comparative example 2: technological process is basically the same as embodiment. The difference is that Soxhlet extraction is used instead of reflux extraction and microwave treatment, and the extraction time is 3 hours. The following steps are the same as the examples.
实施例与比较例的实验结果如表1所示。The experimental results of Examples and Comparative Examples are shown in Table 1.
表1不同方法提取草珊瑚总黄酮的实验结果对比Table 1 Comparison of experimental results of different methods for extracting total flavonoids from Grass coral
实施例与比较例1相比：说明本发明优于传统回流提取工艺。Embodiment and comparative example 1: illustrate that the present invention is better than traditional reflux extraction process.
实施例与比较例2相比：说明本发明优于传统索氏提取工艺。Embodiment compared with comparative example 2: illustrate that the present invention is better than traditional Soxhlet extraction process.
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| CN105622388B (en) * | 2016-04-05 | 2018-03-27 | 惠州学院 | A kind of method of organic acid in buck ultrasonic synergistic extraction plant |
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| Title |
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| 微波萃取技术在中药及天然产物提取中的应用. 傅荣杰，冯怡.中国中药杂志，第28卷第9期. 2003 * |
| 草珊瑚总黄酮提取工艺比较研究. 郁建生，李英伦.江苏农业科学，第5期. 2006 * |
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