阅读说明：本技术 一种滇牡丹果皮提取物及其制备方法和应用 (Paeonia suffruticosa peel extract and preparation method and application thereof ) 是由 施蕊 王娟 杨宇明 于 2020-05-29 设计创作，主要内容包括：本发明涉及生物医药领域,涉及一种中药提取物及其制备方法和应用,具体涉及一种滇牡丹果皮提取物及其制备方法和应用。本方案使用乙酸乙酯对粉碎后的滇牡丹果皮进行热浸提取,通过酸沉处理将黄酮类物质和甾醇类物质分离分层。然后继续对提取后的滤渣进行酶解辅助的热水浸提处理,可以将滇牡丹果皮中的剩余的黄酮类物质和多糖类物质提取。利用本制备方法可同时对滇牡丹果皮中的功效成分进行提取,提高了滇牡丹果皮的综合利用率。本法能够将滇牡丹果皮中的功效成分充分提取利用,可以应用于保健食品的研究开发和生产中。(The invention relates to the field of biological medicines, relates to a traditional Chinese medicine extract, and a preparation method and application thereof, and particularly relates to a paeonia suffruticosa peel extract, and a preparation method and application thereof. According to the scheme, the ethyl acetate is used for carrying out hot-dip extraction on the smashed Yunnan peony peel, and flavonoid substances and sterol substances are separated and layered through acid precipitation treatment. And then carrying out enzymolysis-assisted hot water extraction treatment on the extracted filter residue, so as to extract the residual flavonoid and polysaccharide substances in the paeonia suffruticosa peel. By using the preparation method, the functional components in the Yunnan peony peel can be extracted at the same time, and the comprehensive utilization rate of the Yunnan peony peel is improved. The method can fully extract and utilize the functional components in the Yunnan peony peel, and can be applied to the research, development and production of health-care food.)

1. A preparation method of a paeonia suffruticosa peel extract is characterized by comprising the following steps,

step (1): pretreating Yunnan peony peel to obtain peel particles;

step (2): hot-dipping and extracting the peel particles by using ethyl acetate, filtering after extraction to obtain an extracting solution I and filter residues, and concentrating the extracting solution I to obtain an extract;

and (3): dispersing the extract in water to obtain a dispersion system; adjusting the pH value of the dispersion system to 6.0-6.5, and standing to obtain a precipitate I and an oil layer.

2. The method for preparing the extract of the pericarp of paeonia suffruticosa as claimed in claim 1, further comprising the step (4): and (3) treating the filter residue in the step (2) by using a complex enzyme to obtain an enzymolysis system.

3. The method for preparing the extract of the pericarp of paeonia suffruticosa as claimed in claim 2, further comprising the step (5): adding water into the system after enzymolysis to obtain a water extraction system, adjusting the pH value of the water extraction system to 9.5-10.5, performing hot-dip extraction on the filter residue after enzymolysis, filtering to obtain an extracting solution II after extraction, adjusting the pH value of the extracting solution II to 6.0-6.5, standing, and filtering to obtain a precipitate III and a filtrate.

4. The method for preparing the extract of the pericarp of paeonia suffruticosa as claimed in claim 3, further comprising the step (6): and (5) concentrating the filtrate in the step (5), adding absolute ethyl alcohol, standing, and filtering to obtain a precipitate II.

5. The method for preparing the extract of the pericarp of paeonia suffruticosa as claimed in claim 4, further comprising the step (7): mixing the precipitate I in the step (3) and the precipitate III in the step (6), and then drying to obtain a dry powder flavone extract; removing water from the oil layer in the step (3) to obtain a sterol extract; and (5) drying the precipitate II in the step (5) to obtain a dry powder polysaccharide extract.

6. The method for preparing the extract of the pericarp of paeonia suffruticosa as claimed in claim 5, wherein in the step (2), the temperature for hot-dipping the pericarp particles with ethyl acetate is 40-60 ℃, and the extraction time is 10-15 h.

7. The method for preparing the extract of the pericarp of paeonia suffruticosa as claimed in claim 6, wherein in the step (4), the complex enzyme comprises cellulase, pectinase and protease.

8. The method for preparing the extract of the pericarp of paeonia suffruticosa as claimed in claim 7, wherein in the step (4), the temperature for hot-dipping the filter residue after enzymolysis is 60-70 ℃, and the extraction time is 18-24 h.

9. The paeonia suffruticosa peel extract is characterized by comprising a flavone extract, a sterol extract and a polysaccharide extract.

10. The use of the extract of the pericarp of paeonia suffruticosa as claimed in claim 9 in health food.

Technical Field

The invention relates to the field of biological medicines, relates to a traditional Chinese medicine extract, and a preparation method and application thereof, and particularly relates to a paeonia suffruticosa peel extract, and a preparation method and application thereof.

Background

Paeonia suffruticosa (Paeonia delavayi) is a unique rare or endangered plant in southwest of China, and has high ornamental value and medicinal value. The root bark of the paeonia suffruticosa is the main medicinal part of the paeonia suffruticosa, and the seed oil extracted from the paeonia suffruticosa has the functions of reducing blood fat, reducing blood sugar and the like, so the root bark of the paeonia suffruticosa and the paeonia suffruticosa are widely developed and utilized. However, the pericarp of Paeonia suffruticosa (also called pod) with larger biomass is not comprehensively utilized. Researches show that the pericarp of the paeonia suffruticosa contains a large amount of polysaccharide, sterol (mainly phytosterol) and flavonoid substances. The paeonia suffruticosa polysaccharide can remove hydroxyl free radicals and superoxide anions, has an antioxidant effect, and has high medicinal and health-care values; the sterol has effects of reducing blood lipid, regulating blood lipid, resisting oxidation, relieving inflammation, resisting cancer, and regulating immunity; the flavonoids have antiinflammatory, antiviral, cholagogue, heart tonifying, tranquilizing, and analgesic effects. If various functional components in the Yunnan peony peel can be fully utilized, the application range of the Yunnan peony can be greatly expanded, and the comprehensive utilization of resource species is realized.

The inventor develops an extraction method of the Yunnan peony pericarp polysaccharide in the earlier research results (the extraction process research of the polysaccharide in the pericarp of Yunnan peony which is a national drug, Shili and the like, Chinese national folk medicine, 2016). The method successfully extracts the paeonia suffruticosa peel polysaccharide by using ultrasonic-assisted extraction, reflux method and other extraction methods, and determines the optimal extraction conditions. However, the method in the prior art cannot realize simultaneous extraction of polysaccharide, flavone, sterol and other substances, has limited extraction efficiency, and cannot realize rapid and efficient comprehensive utilization of the pericarp of the paeonia suffruticosa.

Disclosure of Invention

The invention mainly solves the technical problem of providing a preparation method of the paeonia suffruticosa peel extract, by utilizing the preparation method, the functional components in the paeonia suffruticosa peel can be extracted simultaneously, and the comprehensive utilization rate of the paeonia suffruticosa peel is improved.

In order to achieve the purpose, the invention provides the following technical scheme:

a method for preparing extract of pericarp of Paeonia suffruticosa comprises the following steps,

step (1): pretreating Yunnan peony peel to obtain peel particles;

step (2): hot-dipping and extracting the peel particles by using ethyl acetate, filtering after extraction to obtain an extracting solution I and filter residues, and concentrating the extracting solution I to obtain an extract;

and (3): dispersing the extract in water to obtain a dispersion system; adjusting the pH value of the dispersion system to 6.0-6.5, and standing to obtain a precipitate I and an oil layer.

By adopting the technical scheme, the technical principle and the beneficial effects are as follows: hot-soaking and extracting pericarp granule with ethyl acetate to extract sterol substances and part of flavonoids in pericarp granule, and filtering to obtain extractive solution I containing sterol substances and flavonoids. Concentrating the extracting solution I, and volatilizing an extracting solvent ethyl acetate to obtain a semisolid extract. Dispersing the extract in water, wherein the sterol substances are insoluble in water and oily, and standing to collect the sterol substances in the oil layer. And the flavonoid substance has poor water solubility and is easy to form crystal precipitation. Adjusting pH to 6.0-6.5 to ensure that flavonoids are fully separated out to obtain precipitate I.

The inventors have tried a number of different extraction methods, for example, ultrasonic assisted extraction of peel particles using ethyl acetate. It is well known that ultrasound-assisted extraction has higher extraction efficiency, shorter time, and higher extraction efficiency of the effective substances than thermal extraction. However, in the actual situation, the amount of sterols obtained by extraction is small and the purity of flavonoids is not high by using the ultrasonic-assisted extraction method. The inventor analyzes the reason of the phenomenon, and considers that the flavone to be extracted by the method is the total flavone in the Yunnan peony peel, and the components are relatively complex. Some flavonoids have inclusion effect on sterol substances in the process of precipitation and crystallization, and the precipitation carries partial sterol and other substances, so the phenomenon is caused. In the course of attempting various extraction methods, the inventors have found that the yield of sterols can be improved by the hot-dip extraction method, and the purity of flavonoids can be improved although the amount of flavonoids obtained is not high. The inventors further analyzed the cause: the phytosterol exists on plant cell membranes, and is easily dissolved out by a solvent through different extraction methods (simple hot dipping treatment, ultrasonic assisted extraction and the like); while flavonoids in the fruit skin of the paeonia suffruticosa are distributed more complexly, some flavonoids are combined with the structural skeleton part in plant cells more tightly (the flavonoids can be extracted by a stronger extraction method), and some flavonoids are free in cytoplasm (the flavonoids can be obtained by a general extraction method). When the ultrasonic-assisted extraction method is adopted, flavonoids are fully extracted, but when substances such as sterol and the like are separated, functional components cannot be fully separated. When hot-dipping extraction is adopted, only part of flavonoids are extracted, and the flavonoids do not have inclusion effect (or have small inclusion effect) on the sterols, so that the extraction rate of the sterols is improved, and the purity of the flavonoids is improved. And the hot-dipping extraction method is adopted, so that the dissolved impurities are less, and the purity of the target substance is improved.

By adopting the technical scheme, the sterol substances and the flavonoid substances can be extracted and obtained simultaneously, the yield of the sterol substances is higher, and the purity of the flavonoid substances is higher. In addition, the inventor finds out one of the important factors influencing the extraction rate of the sterol substances, and can avoid the influence of another target substance on the extraction rate of the sterol substances by simply adjusting the extraction method.

And (3) further comprising a step (4) of treating the filter residue in the step (2) by using complex enzyme to obtain an enzymolysis system.

By adopting the technical scheme, the filter residue can be fully utilized. After the filter residue is treated by the compound enzyme, the cell wall can be disintegrated, which is beneficial to fully extracting the functional components in the cells.

Further, the method also comprises the step (5): adding water into the system after enzymolysis to obtain a water extraction system, adjusting the pH value of the water extraction system to 9.5-10.5, performing hot-dip extraction on the filter residue after enzymolysis, filtering to obtain an extracting solution II after extraction, adjusting the pH value of the extracting solution II to 6.0-6.5, standing, and filtering to obtain a precipitate III and a filtrate.

By adopting the technical scheme, the functional substances including total polysaccharide and partial flavone in the filter residue can be fully extracted. The pH value is adjusted to enable flavonoid substances extracted from the filter residue to be precipitated and crystallized, so that the separation and purification of the flavonoid substances are realized.

Further, the method also comprises the step (6): and (5) concentrating the filtrate in the step (5), adding absolute ethyl alcohol, standing, and filtering to obtain a precipitate II.

By adopting the technical scheme, the polysaccharide precipitate is purified and separated by using an alcohol precipitation method.

Further, the method also comprises the step (7): mixing the precipitate I in the step (3) and the precipitate III in the step (6), and then drying to obtain a dry powder flavone extract; removing water from the oil layer in the step (3) to obtain a sterol extract; and (5) drying the precipitate II in the step (5) to obtain a dry powder polysaccharide extract.

By adopting the technical scheme, the flavone extract, the sterol extract and the polysaccharide extract which have high purity and are easy to preserve can be obtained through dehydration or drying treatment. And mixing the precipitate I and the precipitate III to obtain the total flavonoids in the pericarp of the paeonia suffruticosa so as to realize the full extraction of the flavonoids.

Further, in step (2), hot-dipping extraction of the pericarp particles with ethyl acetate is carried out at 40-60 deg.C for 10-15 h.

By adopting the technical scheme and the temperature and time, the sterol substances can be fully extracted, and partial flavonoid substances which influence the layering and precipitation of the sterol cannot be extracted.

Further, in the step (4), the complex enzyme comprises cellulase, pectinase and protease.

By adopting the technical scheme, the cellulase, the pectinase and the protease can fully degrade the plant cell wall, so that the content is fully separated out.

Further, in the step (4), the temperature for hot-dipping extraction of the filter residue after enzymolysis is 60-70 ℃, and the extraction time is 18-24 h.

By adopting the technical scheme and the temperature and time, the total polysaccharide and the residual flavonoid can be fully extracted.

Further, the paeonia suffruticosa peel extract comprises a flavone extract, a sterol extract and a polysaccharide extract.

By adopting the technical scheme, the extract of the pericarp of the paeonia suffruticosa obtained by the method comprises three types of flavone extract, sterol extract and polysaccharide extract, so that the comprehensive utilization of the pericarp of the paeonia suffruticosa and the full extraction of functional components are realized.

Further, the extract of the pericarp of the paeonia suffruticosa is applied to health-care food.

By adopting the technical scheme, the flavone extract of the paeonia suffruticosa has the effects of anti-inflammation, antivirus and the like; the active polysaccharide of the paeonia suffruticosa has the effects of resisting oxidation, activating an immune system and the like; the sterol extract of the paeonia suffruticosa has application values of lipid lowering, lipid regulating, oxidation resistance and the like, and the paeonia suffruticosa peel extract can be applied to research, development and production of health-care food.

Detailed Description