WO2017185281A1 - 一种贝母花提取物的制备方法 - Google Patents
一种贝母花提取物的制备方法 Download PDFInfo
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- WO2017185281A1 WO2017185281A1 PCT/CN2016/080473 CN2016080473W WO2017185281A1 WO 2017185281 A1 WO2017185281 A1 WO 2017185281A1 CN 2016080473 W CN2016080473 W CN 2016080473W WO 2017185281 A1 WO2017185281 A1 WO 2017185281A1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8966—Fritillaria, e.g. checker lily or mission bells
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- the invention relates to the field of biological extraction technology, in particular to a preparation method of a fritillaria flower extract.
- the fritillary flowers are perennial herbs, and the underground part is a bulb composed of two scales. Stems erect, about 50 cm high, leaves broadly linear, apex narrow, sometimes vine-like entangled, 3 to 4 rounds. From April to May, the bell-shaped pale yellow flowers will hang from the sides of the leaves on the upper part of the leaves. Pick when the bottom two flowers of Zhebei plant are open.
- Fritillaria has a cough and phlegm-reducing effect, can be used for colds, bronchitis caused by cough, sore throat, with its bulbs have a pharmacological effect.
- the present invention proposes a preparation method of a fritillaria flower extract, which has high extraction speed and extraction precision, and low production cost.
- the method for preparing a fritillaria flower extract proposed by the invention comprises the following steps:
- the resin After mixing the extract and the extract, the resin is adsorbed on the macropores, and then eluted with water and an aqueous solution of ethanol, concentrated, and dried to obtain an extract of Fritillaria.
- the temperature for drying at a low temperature is 10 to 20 ° C
- the pressure for drying at a low temperature is 5 to 10 Pa
- the time for drying at a low temperature is 25 to 28 hours.
- the ultrasonic extraction power is 500 to 600 w
- the ultrasonic extraction frequency is 50 to 60 kHz
- the ultrasonic extraction time is 3 to 4 h.
- the supercritical extraction conditions are: an extraction temperature of 52 to 55 ° C, a first separation temperature of 45 to 50 ° C, a second separation temperature of 35 to 40 ° C, an extraction pressure of 30 to 33 MPa, and carbon dioxide.
- the flow rate is 10-20 L/h
- the frequency of the received product is 45-50 min/time
- the extraction time is 3-4 h.
- the ratio of material to liquid is 1:10 to 12
- the pH of the solution is 3 to 5.
- the concentration of the aqueous ethanol solution in S3 is 50 to 60%, and the concentration of the aqueous ethanol solution in S4 is 40 to 50%.
- Ultrasonic extraction can produce strong vibration, high acceleration, strong cavitation and agitation. When used for solvent-assisted extraction, it can accelerate the extract of Fritillaria flower into the solvent, thus shortening the extraction time, saving solvent and avoiding the high temperature leading to the extraction of Fritillaria. Decomposition of the material, but the purity of the extract of Fritillaria frondosa obtained by ultrasonic extraction is insufficient, and the residual rate in the residue is high; while the purity of the extract of Fritillaria flower extract obtained by supercritical carbon dioxide extraction is above 85%, which can satisfy various kinds of extracts containing Fritillaria.
- the development needs of foods, health products and medicines of ingredients can also be used as pharmaceutical intermediates, but the extraction speed is often slow.
- the invention adopts ultrasonic extraction and supercritical carbon dioxide extraction for series connection, which not only improves the extraction speed and extraction precision, but also greatly reduces the production cost, and extracts the fritillary flower extract extracted from the fritillary flower for the related enterprises to develop and produce a tumor for prevention and treatment.
- Medicines and health foods that reduce blood sugar, protect liver and gallbladder, etc. provide high-quality raw materials for production.
- the method for preparing a fritillaria flower extract proposed by the invention comprises the following steps:
- the fritillary flower is dried at a low temperature
- the temperature of low temperature drying is 10 ° C
- the pressure of low temperature drying is 10 Pa
- the drying time of low temperature is 25 h, crushing, sieving, and then degreasing to obtain a filter cake
- the ultrasonic extraction power is 600w
- the frequency of ultrasonic extraction is 50 kHz
- the ultrasonic extraction time is 4 h
- the extract and the residue are obtained by filtration;
- the supercritical extraction conditions are: extraction temperature is 55 ° C, first separation temperature is 45 ° C, second separation The temperature is 40 ° C, the extraction pressure is 30 MPa, the carbon dioxide flow rate is 20 L / h, the frequency of the received product is 45 min / time, the extraction time is 4 h;
- the macroporous adsorption resin is used, the ratio of material to liquid is 1:10, the pH of the solution is 5, and then eluted with water and a 40% aqueous solution of ethanol, concentrated, and dried. A flower of the fritillaria is obtained.
- the method for preparing a fritillaria flower extract proposed by the invention comprises the following steps:
- the fritillary flower is dried at a low temperature
- the temperature of low temperature drying is 20 ° C
- the pressure of low temperature drying is 5 Pa
- the time of low temperature drying is 28 h, pulverization, sieving, and then degreasing to obtain a filter cake
- the ultrasonic extraction power is 500w
- the frequency of ultrasonic extraction is 60 kHz
- the ultrasonic extraction time is 3 h
- the extract and the residue are obtained by filtration;
- the supercritical extraction conditions are: extraction temperature is 52 ° C, first separation temperature is 50 ° C, second separation The temperature is 35 ° C, the extraction pressure is 33 MPa, the carbon dioxide flow rate is 10 L / h, the frequency of the received product is 50 min / time, the extraction time is 3 h;
- the macroporous adsorption resin After mixing the extract and the extract, the macroporous adsorption resin is used, the ratio of material to liquid is 1:12, the pH of the solution is 3, and then eluted with water and a 50% aqueous solution of ethanol, concentrated, and dried. A flower of the fritillaria is obtained.
- the method for preparing a fritillaria flower extract proposed by the invention comprises the following steps:
- the fritillary flower is dried at a low temperature
- the temperature of low temperature drying is 15 ° C
- the pressure of low temperature drying is 8 Pa
- the drying time of low temperature is 26 h, crushing, sieving, and then degreasing to obtain a filter cake
- ultrasonic extraction is carried out by adding absolute ethanol, the ultrasonic extraction power is 580w, the ultrasonic extraction frequency is 53 kHz, the ultrasonic extraction time is 3.7 h, and then the extract and the residue are obtained by filtration;
- the residue is subjected to supercritical carbon dioxide extraction to obtain an extract, and the concentration of 54% ethanol aqueous solution is used as an entrainer.
- the supercritical extraction conditions are: extraction temperature is 54 ° C, first separation temperature is 46 ° C, second separation The temperature is 37 ° C, the extraction pressure is 31 MPa, the carbon dioxide flow rate is 18 L / h, the frequency of the received product is 46 min / time, the extraction time is 3.4 h;
- the macroporous adsorption resin After mixing the extract and the extract, the macroporous adsorption resin is used, the ratio of material to liquid is 1:11, the pH of the solution is 4, and then eluted with water and a 45% aqueous solution of ethanol, concentrated, and dried. Get Fritillaria flower extract.
- the method for preparing a fritillaria flower extract proposed by the invention comprises the following steps:
- the fritillary flower is dried at a low temperature
- the temperature of low temperature drying is 18 ° C
- the pressure of low temperature drying is 6 Pa
- the time of low temperature drying is 27 h, crushing, sieving, and then degreasing to obtain a filter cake
- the ultrasonic extraction power is 550w
- the frequency of ultrasonic extraction is 56kHz
- the ultrasonic extraction time is 3.3h
- the extract and the residue are filtered
- the supercritical extraction conditions are: extraction temperature is 53 ° C, first separation temperature is 48 ° C, second separation The temperature is 36 ° C, the extraction pressure is 32 MPa, the carbon dioxide flow rate is 12 L / h, the frequency of the received product is 48 min / time, the extraction time is 3.2 h;
- the macroporous adsorption resin After mixing the extract and the extract, the macroporous adsorption resin is used, the ratio of material to liquid is 1:11, the pH of the solution is 4, and then eluted with water and a 45% aqueous solution of ethanol, concentrated, and dried. A flower of the fritillaria is obtained.
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
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Abstract
一种贝母花提取物的制备方法，包括如下步骤：将贝母花低温干燥后，粉碎，过筛，接着脱脂得到滤饼；将滤饼干燥后，加入无水乙醇中进行超声提取，接着过滤得到提取液和残渣；将残渣进行超临界二氧化碳萃取得到萃取液，以乙醇水溶液为夹带剂；将萃取液和提取液混合后，上大孔吸附树脂，然后依次采用水和乙醇水溶液洗脱，浓缩，干燥，得到贝母花提取物。超临界萃取中，萃取温度为52～55℃，第一次分离温度为45～50℃，第二次分离温度为35～40℃，萃取压力为30～33MPa，二氧化碳流速为10～20L/h，接收产物的频率为45～50min/次，提取时间为3～4h。该制备方法提取速度和提取精度高，生产成本低。
Description
本发明涉及生物提取技术领域，尤其涉及一种贝母花提取物的制备方法。
贝母花多年生草本，地下部分为二鳞片组成的球茎。茎直立，高约50公分，叶宽线形，先端细窄，有时会会呈藤蔓状缠绕，3～4枚轮生。4～5月时，会从上面部分的叶子两侧垂下吊钟形淡黄色花，观赏性佳。当浙贝植株最下两朵花开放时采摘。
贝母花有止咳化痰作用，能用于感冒、支气管炎引起的咳嗽、喉咙痛，用其鳞茎有药效作用。
发明内容
基于背景技术存在的技术问题，本发明提出了一种贝母花提取物的制备方法，不仅提取速度和提取精度高，而且生产成本低。
本发明提出的一种贝母花提取物的制备方法，包括如下步骤：
S1、将贝母花低温干燥后，粉碎，过筛，接着脱脂得到滤饼；
S2、将滤饼干燥后，加入无水乙醇中进行超声提取，接着过滤得到提取液和残渣；
S3、将残渣进行超临界二氧化碳萃取得到萃取液，以乙醇水溶液为夹带剂；
S4、将萃取液和提取液混合后，上大孔吸附树脂，然后依次采用水和乙醇水溶液洗脱，浓缩，干燥，得到贝母花提取物。
进一步地，S1中，低温干燥的温度为10～20℃，低温干燥的压力为5～10Pa，低温干燥的时间为25～28h。
进一步地，S2中，超声提取的功率为500～600w，超声提取的频率为50～60kHz，超声提取的时间为3～4h。
进一步地，S3中，超临界萃取条件为：萃取温度为52～55℃，第一次分离温度为45～50℃，第二次分离温度为35～40℃，萃取压力为30～33MPa，二氧化碳流速为10～20L/h，接收产物的频率为45～50min/次，提取时间为3～4h。
进一步地，S4的上大孔吸附树脂过程中，料液比为1：10～12，溶液的pH值为3～5。
进一步地，S3中的乙醇水溶液浓度为50～60％，S4中的乙醇水溶液浓度40～50％。
超声提取可以产生强烈振动、高加速度、强烈空化作用及搅拌作用，用于溶剂辅助提取时，可以加速贝母花提取物进入溶剂，从而缩短提取时间、节约溶剂，避免高温导致贝母花提取物分解，但超声提取得到的贝母花提取物纯度不足，残渣中残留率高；而超临界二氧化碳萃取得到的贝母花提取物纯度在85％以上，可满足各种对含有贝母花提取物成分的食品、保健品和药物的开发需求，亦可作为药物中间体使用，但往往提取速度慢。
本发明采用超声提取和超临界二氧化碳萃取进行串联，不仅提高了提取速度和提取精度，而且大大降低了生产成本，从贝母花中提取的贝母花提取物为相关企业开发生产预防和治疗肿瘤、降低血糖、保肝利胆等作用的药品和保健食品提供了优质生产原料。
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例1
本发明提出的一种贝母花提取物的制备方法，包括如下步骤：
S1、将贝母花低温干燥，低温干燥的温度为10℃，低温干燥的压力为10Pa，低温干燥的时间为25h，粉碎，过筛，接着脱脂得到滤饼；
S2、将滤饼干燥后，加入无水乙醇中进行超声提取，超声提取的功率为600w，超声提取的频率为50kHz，超声提取的时间为4h，接着过滤得到提取液和残渣；
S3、将残渣进行超临界二氧化碳萃取得到萃取液，以浓度为50％的乙醇水溶液为夹带剂，超临界萃取条件为：萃取温度为55℃，第一次分离温度为45℃，第二次分离温度为40℃，萃取压力为30MPa，二氧化碳流速为20L/h，接收产物的频率为45min/次，提取时间为4h；
S4、将萃取液和提取液混合后，上大孔吸附树脂，料液比为1：10，溶液的pH值为5，然后依次采用水和浓度40％的乙醇水溶液洗脱，浓缩，干燥，得到贝母花提取物。
实施例2
本发明提出的一种贝母花提取物的制备方法，包括如下步骤：
S1、将贝母花低温干燥，低温干燥的温度为20℃，低温干燥的压力为5Pa，低温干燥的时间为28h，粉碎，过筛，接着脱脂得到滤饼；
S2、将滤饼干燥后，加入无水乙醇中进行超声提取，超声提取的功率为500w，超声提取的频率为60kHz，超声提取的时间为3h，接着过滤得到提取液和残渣；
S3、将残渣进行超临界二氧化碳萃取得到萃取液，以浓度为60％的乙醇水溶液为夹带剂，超临界萃取条件为：萃取温度为52℃，第一次分离温度为50℃，第二次分离温度为35℃，萃取压力为33MPa，二氧化碳流速为10L/h，接收产物的频率为50min/次，提取时间为3h；
S4、将萃取液和提取液混合后，上大孔吸附树脂，料液比为1：12，溶液的pH值为3，然后依次采用水和浓度50％的乙醇水溶液洗脱，浓缩，干燥，得到贝母花提取物。
实施例3
本发明提出的一种贝母花提取物的制备方法，包括如下步骤：
S1、将贝母花低温干燥，低温干燥的温度为15℃，低温干燥的压力为8Pa，低温干燥的时间为26h，粉碎，过筛，接着脱脂得到滤饼；
S2、将滤饼干燥后，加入无水乙醇中进行超声提取，超声提取的功率为580w，超声提取的频率为53kHz，超声提取的时间为3.7h，接着过滤得到提取液和残渣；
S3、将残渣进行超临界二氧化碳萃取得到萃取液，以浓度为54％的乙醇水溶液为夹带剂，超临界萃取条件为：萃取温度为54℃，第一次分离温度为46℃，第二次分离温度为37℃，萃取压力为31MPa，二氧化碳流速为18L/h，接收产物的频率为46min/次，提取时间为3.4h；
S4、将萃取液和提取液混合后，上大孔吸附树脂，料液比为1：11，溶液的pH值为4，然后依次采用水和浓度45％的乙醇水溶液洗脱，浓缩，干燥，得到
贝母花提取物。
实施例4
本发明提出的一种贝母花提取物的制备方法，包括如下步骤：
S1、将贝母花低温干燥，低温干燥的温度为18℃，低温干燥的压力为6Pa，低温干燥的时间为27h，粉碎，过筛，接着脱脂得到滤饼；
S2、将滤饼干燥后，加入无水乙醇中进行超声提取，超声提取的功率为550w，超声提取的频率为56kHz，超声提取的时间为3.3h，接着过滤得到提取液和残渣；
S3、将残渣进行超临界二氧化碳萃取得到萃取液，以浓度为56％的乙醇水溶液为夹带剂，超临界萃取条件为：萃取温度为53℃，第一次分离温度为48℃，第二次分离温度为36℃，萃取压力为32MPa，二氧化碳流速为12L/h，接收产物的频率为48min/次，提取时间为3.2h；
S4、将萃取液和提取液混合后，上大孔吸附树脂，料液比为1：11，溶液的pH值为4，然后依次采用水和浓度45％的乙醇水溶液洗脱，浓缩，干燥，得到贝母花提取物。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (10)
- 一种贝母花提取物的制备方法，其中，包括如下步骤：S1、将贝母花低温干燥后，粉碎，过筛，接着脱脂得到滤饼；S2、将滤饼干燥后，加入无水乙醇中进行超声提取，接着过滤得到提取液和残渣；S3、将残渣进行超临界二氧化碳萃取得到萃取液，以乙醇水溶液为夹带剂；S4、将萃取液和提取液混合后，上大孔吸附树脂，然后依次采用水和乙醇水溶液洗脱，浓缩，干燥，得到贝母花提取物。
- 根据权利要求1所述贝母花提取物的制备方法，其中，S1中，低温干燥的温度为10～20℃，低温干燥的压力为5～10Pa，低温干燥的时间为25～28h。
- 根据权利要求1所述贝母花提取物的制备方法，其中，S2中，超声提取的功率为500～600w，超声提取的频率为50～60kHz，超声提取的时间为3～4h。
- 根据权利要求1所述贝母花提取物的制备方法，其中，S3中，超临界萃取条件为：萃取温度为52～55℃，第一次分离温度为45～50℃，第二次分离温度为35～40℃，萃取压力为30～33MPa，二氧化碳流速为10～20L/h，接收产物的频率为45～50min/次，提取时间为3～4h。
- 根据权利要求1所述贝母花提取物的制备方法，其中，S4的上大孔吸附树脂过程中，料液比为1：10～12，溶液的pH值为3～5。
- 根据权利要求1所述贝母花提取物的制备方法，其中，S3中的乙醇水溶液浓度为50～60％，S4中的乙醇水溶液浓度40～50％。
- 根据权利要求2所述贝母花提取物的制备方法，其中，S2中，超声提取的功率为500～600w，超声提取的频率为50～60kHz，超声提取的时间为3～4h。
- 根据权利要求7所述贝母花提取物的制备方法，其中，S3中，超临界萃取条件为：萃取温度为52～55℃，第一次分离温度为45～50℃，第二次分离温度为35～40℃，萃取压力为30～33MPa，二氧化碳流速为10～20L/h，接收产物的频率为45～50min/次，提取时间为3～4h。
- 根据权利要求8所述贝母花提取物的制备方法，其中，S4的上大孔吸附树脂过程中，料液比为1：10～12，溶液的pH值为3～5。
- 根据权利要求9所述贝母花提取物的制备方法，其中，S3中的乙醇水溶液浓度为50～60％，S4中的乙醇水溶液浓度40～50％。
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| PCT/CN2016/080473 WO2017185281A1 (zh) | 2016-04-28 | 2016-04-28 | 一种贝母花提取物的制备方法 |
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