CN101708215B - A method for extracting triterpenoids from Schisandra chinensis - Google Patents
A method for extracting triterpenoids from Schisandra chinensis Download PDFInfo
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- 235000008422 Schisandra chinensis Nutrition 0.000 title claims abstract description 43
- 240000006079 Schisandra chinensis Species 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 17
- 150000003648 triterpenes Chemical class 0.000 title claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000000284 extract Substances 0.000 claims abstract description 13
- 108010059892 Cellulase Proteins 0.000 claims abstract description 9
- 229940106157 cellulase Drugs 0.000 claims abstract description 9
- 238000010262 high-speed countercurrent chromatography Methods 0.000 claims abstract description 9
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 31
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 241000736075 Schisandra Species 0.000 claims description 10
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000011344 liquid material Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 239000012488 sample solution Substances 0.000 claims description 5
- XBZYWSMVVKYHQN-MYPRUECHSA-N (4as,6as,6br,8ar,9r,10s,12ar,12br,14bs)-10-hydroxy-2,2,6a,6b,9,12a-hexamethyl-9-[(sulfooxy)methyl]-1,2,3,4,4a,5,6,6a,6b,7,8,8a,9,10,11,12,12a,12b,13,14b-icosahydropicene-4a-carboxylic acid Chemical compound C1C[C@H](O)[C@@](C)(COS(O)(=O)=O)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C XBZYWSMVVKYHQN-MYPRUECHSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 2
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000002137 ultrasound extraction Methods 0.000 abstract description 4
- 239000013543 active substance Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000197 pyrolysis Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 9
- 230000005526 G1 to G0 transition Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 229930013686 lignan Natural products 0.000 description 2
- 150000005692 lignans Chemical class 0.000 description 2
- 235000009408 lignans Nutrition 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000004227 thermal cracking Methods 0.000 description 2
- 241000345998 Calamus manan Species 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 235000012950 rattan cane Nutrition 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种从北五味子中提取三萜类物质的方法，具体的是涉及一种利用组织破碎、纤维素酶和超声萃取前处理物料，并利用超临界流体萃取技术结合高速逆流色谱技术分离提取出北五味子三萜类物质，为北五味子三萜类物质的分离纯化提供一种有效的方法。The invention relates to a method for extracting triterpenoids from Schisandra chinensis, in particular to a method for pretreatment of materials by tissue crushing, cellulase and ultrasonic extraction, and separation by supercritical fluid extraction technology combined with high-speed countercurrent chromatography technology The extraction of triterpenoids from Schisandra chinensis provides an effective method for the separation and purification of triterpenoids from Schisandra chinensis.
背景技术Background technique
五味子属隶属于五味子科，约27种，在我国除新疆、青海、海南外各省区都有分布，其中约19种可供药用，药用价值最大的是五味子(习称“北五味子”)，其次是华中五味子(习称“南五味子”)。其中北五味子药用价值极高，具有抗病毒、抗肿瘤、提高人体免疫力等功效。它包含多种功效成分，其中主要是木脂素、多糖和三萜类化合物。而目前国内外对五味子研究多集中在南五味子，功能性成分研究业集中在木脂素类和多糖类物质上，而关于北五味子三萜类物质提取报道较少，多数报道集中在结构鉴定和功能性方面。The genus Schisandra belongs to the family Schisandra, and there are about 27 species, which are distributed in all provinces and regions in my country except Xinjiang, Qinghai, and Hainan. Among them, about 19 species are available for medicinal use, and the most medicinal value is Schisandra (commonly known as "Northern Schisandra") , followed by Huazhong Schisandra (commonly known as "Southern Schisandra"). Among them, the medicinal value of Schisandra chinensis is extremely high, and it has the effects of anti-virus, anti-tumor, and improving human immunity. It contains a variety of functional components, mainly lignans, polysaccharides and triterpenoids. At present, the research on Schisandra chinensis at home and abroad is mostly concentrated on southern Schisandra chinensis, and the research on functional components is concentrated on lignans and polysaccharides. However, there are few reports on the extraction of triterpenoids from northern Schisandra chinensis, and most reports focus on structural identification. and functional aspects.
目前北五味子三萜提取方法，多集中在乙醇或者丙酮溶液回流提取法，此法操作过程繁杂，物料受热温度高，三萜类物质损失严重，提取率较低。现在，三萜类物质的分离与纯化通常采用柱色谱法，样品在固定相的吸附导致回收率很低。At present, the triterpenoid extraction methods of Schisandra chinensis mainly focus on the reflux extraction method of ethanol or acetone solution. The operation process of this method is complicated, the heating temperature of the material is high, the loss of triterpenoids is serious, and the extraction rate is low. At present, the separation and purification of triterpenoids usually use column chromatography, and the adsorption of the sample on the stationary phase leads to a very low recovery rate.
发明内容Contents of the invention
本发明的目的是利用组织破碎、纤维素酶和超声萃取前处理物料，并利用超临界流体萃取技术结合高速逆流色谱技术分离提取出北五味子三萜类物质，提取率比常规溶剂提取法提高10-15％，而且操作过程简单，能耗低，无污染，回收率高，避免萃取物在高温下热裂解，保护生理活性物质的活性。The purpose of the present invention is to use tissue crushing, cellulase and ultrasonic extraction to pre-treat materials, and use supercritical fluid extraction technology combined with high-speed countercurrent chromatography to separate and extract triterpenoids from Schisandra chinensis, and the extraction rate is 10 times higher than that of conventional solvent extraction methods. -15%, and the operation process is simple, low energy consumption, no pollution, high recovery rate, avoid thermal cracking of the extract at high temperature, and protect the activity of physiologically active substances.
本发明提供的技术方案是：The technical scheme provided by the invention is:
以北五味子藤茎为主要原料，先将原料切成1cm-2cm长度后放入高速组织匀浆捣碎机中，在12000rpm条件下保持15min后，按照液料比为13mL/1g的比例加入浓度80％的氯仿溶液后，再加入按照北五味子藤茎原料重量比为0.5％的纤维素酶，在超声功率600W、40℃条件下，酶解20min后，再在75℃恒温干燥18h，粉碎过60目筛为粉末备用；With the cane of Schisandra chinensis as the main raw material, first cut the raw material into 1cm-2cm length, put it into a high-speed tissue homogenizer, keep it at 12000rpm for 15min, and then add the concentration according to the ratio of liquid to material 13mL/1g After adding 80% chloroform solution, add 0.5% cellulase according to the weight ratio of Schisandra chinensis rattan raw material, under the condition of ultrasonic power 600W and 40°C, after enzymolysis for 20min, then dry at 75°C for 18h, and pulverize 60 mesh sieve is used for powder;
取过筛后粉末200-300g加入到超临界萃取釜中，设定萃取温度46℃、分离温度55℃开始萃取加压，调节CO2流量恒定在18L/h，萃取釜压力恒定在18MPa后，启动夹带剂泵，按照液料比为0.8mL/1g比例、浓度为85％乙酸乙酯和液料比为0.2mL/1g、浓度为80％乙醇组成的复合夹带剂混匀后，打入夹带剂釜，萃取135min后，收集北五味子萃取液，减压回收溶剂，真空干燥为干燥粉末备用；Take 200-300g of the sieved powder and add it to the supercritical extraction kettle, set the extraction temperature to 46°C, and the separation temperature to 55°C to start the extraction and pressurize, adjust the CO2 flow to be constant at 18L/h, and the pressure of the extraction kettle to be constant at 18MPa, Start the entrainer pump, mix the compound entrainer composed of 0.8mL/1g liquid-to-material ratio, 85% ethyl acetate and 0.2mL/1g liquid-to-solid ratio, and 80% ethanol, and inject it into the entrainer After extraction for 135 minutes, collect the extract of Schisandra chinensis, recover the solvent under reduced pressure, and vacuum-dry to prepare dry powder for later use;
称取真空干燥后粉末，加入按照液料比为10mL/1g、浓度为80％正丙醇，液料比为8mL/1g、浓度为75％乙酸乙酯，液料比为6mL/1g、浓度为90％氯仿，液料比为10mL/1g纯净水组成的复合溶剂中，在分液漏斗中平衡24h后，使用前分离成上相和下相，分别脱气后备用；Weigh the powder after vacuum drying, add n-propanol according to the liquid-solid ratio of 10mL/1g, the concentration is 80%, the liquid-solid ratio is 8mL/1g, the concentration is 75% ethyl acetate, the liquid-solid ratio is 6mL/1g, the concentration In a composite solvent composed of 90% chloroform and a liquid-to-solid ratio of 10mL/1g pure water, after equilibrating in a separatory funnel for 24 hours, separate into an upper phase and a lower phase before use, and degas respectively for later use;
取上下相配制成样品溶液，注入高速逆流色谱，转速为850r/min，流量为3.5mL/min，检测波长为254nm，时间为135-180min，收集流出液，进行浓缩、干燥，制得北五味子三萜粉末。Take the upper and lower phases to prepare a sample solution, inject it into high-speed countercurrent chromatography, the rotation speed is 850r/min, the flow rate is 3.5mL/min, the detection wavelength is 254nm, and the time is 135-180min. The effluent is collected, concentrated and dried to obtain Schisandra chinensis Triterpene powder.
本发明利用组织破碎、纤维素酶和超声萃取前处理物料，并利用超临界流体萃取技术结合高速逆流色谱技术分离提取出北五味子三萜类物质，其优点是：1、提取率较常规溶剂提取法明显提高；2、操作过程简单，能耗低，对生产环境无污染；3、回收率高，避免了萃取物在高温下热裂解，保护生理活性物质的活性；4工艺技术简单，成本低廉，易于工业化生产。The present invention uses tissue crushing, cellulase and ultrasonic extraction to pre-treat materials, and uses supercritical fluid extraction technology combined with high-speed countercurrent chromatography to separate and extract triterpenoids from Schisandra chinensis. The advantages are: 1. The extraction rate is higher than that of conventional solvent extraction 2. The operation process is simple, the energy consumption is low, and there is no pollution to the production environment; 3. The recovery rate is high, which avoids the thermal cracking of the extract at high temperature and protects the activity of physiologically active substances; 4. The process technology is simple and the cost is low , easy to industrial production.
具体实施方式Detailed ways
实施例1Example 1
北五味子藤茎1000g，先将原料切成1cm长度后放入高速组织匀浆捣碎机在12000rpm条件下保持15min后，按照液料比[溶剂体积(mL)/原料重量(g)]13mL∶1g加入浓度80％氯仿溶液13000mL后，再加入原料重量比为0.5％纤维素酶5g(酶活力为40000U/g，食品级)，在超声功率600W，40℃条件下，酶解20min后，再在75℃恒温干燥18h，粉碎过60目筛为粉末备用。Schisandra chinensis cane 1000g, first cut the raw material into 1cm length and then put it into a high-speed tissue homogenizer and grinder, keep it for 15min under the condition of 12000rpm, according to the ratio of liquid to material [volume of solvent (mL)/weight of raw material (g)] 13mL: After adding 1 g of 13000 mL of 80% chloroform solution, 5 g of cellulase (enzyme activity of 40000 U/g, food grade) with a weight ratio of 0.5% of the raw material was added, and after 20 min of enzymolysis at 600 W of ultrasonic power and 40 ° C, the Dry at a constant temperature of 75°C for 18 hours, crush and pass through a 60-mesh sieve as powder for future use.
取过筛后粉末200g加入到超临界萃取釜中，设定萃取温度46℃、分离器温度55℃开始萃取加压，调节CO2流量恒定在18L/h，萃取釜压力恒定在18MPa后，启动夹带剂泵，按照液料比[溶剂体积(mL)/过筛后粉末重量(g)]为0.8mL∶1g、浓度为85％乙酸乙酯160mL和液料比为0.2mL∶1g、浓度为80％乙醇40mL组成的复合夹带剂混匀后，打入夹带剂釜，萃取135min后，收集北五味子萃取液，减压回收溶剂，真空干燥为干燥粉末备用。Take 200g of the sieved powder and put it into the supercritical extraction kettle, set the extraction temperature to 46°C and the temperature of the separator to 55°C to start extraction and pressurization, adjust the CO2 flow to be constant at 18L/h, and the pressure of the extraction kettle to be constant at 18MPa, start Entrainer pump, according to the ratio of liquid to material [volume of solvent (mL)/weight of powder after sieving (g)] is 0.8mL: 1g, concentration is 85% ethyl acetate 160mL and ratio of liquid to material is 0.2mL: 1g, concentration is After mixing the compound entrainer composed of 40mL of 80% ethanol, put it into the entrainer tank, extract for 135min, collect the extract of Schisandra chinensis, recover the solvent under reduced pressure, and dry it in vacuum to obtain a dry powder for later use.
称取真空干燥后粉末10g，加入按照液料比[溶剂体积(mL)/真空干燥后粉末重量(g)]为10mL∶1g、浓度为80％正丙醇100mL，液料比为8mL∶1g浓度为75％乙酸乙酯80mL，液料比为6mL∶1g、浓度为90％氯仿60mL，液料比为10mL∶1g纯净水100mL组成的复合溶剂中，在分液漏斗中平衡24h后，使用前分离成上相(固定相)和下相(流动相)，分别脱气后备用，取上下相配制成样品溶液，注入高速逆流色谱，选择转速850r/min、流量3.5mL/min、检测波长为254nm、收集时间135-180min，对流出液进行浓缩、干燥，制得北五味子三萜粉末。Weigh 10g of the powder after vacuum drying, add 10mL: 1g according to the liquid-material ratio [solvent volume (mL)/powder weight after vacuum drying (g)], the concentration is 80% n-propanol 100mL, the liquid-material ratio is 8mL: 1g Concentration is 75% ethyl acetate 80mL, liquid-solid ratio is 6mL: 1g, concentration is 90% chloroform 60mL, liquid-solid ratio is 10mL: 1g in the compound solvent that pure water 100mL forms, after equilibrating in separating funnel 24h, use Separated into upper phase (stationary phase) and lower phase (mobile phase) before, degassed separately and then used for later use, take upper and lower phases to prepare sample solution, inject high-speed countercurrent chromatography, select speed 850r/min, flow rate 3.5mL/min, detection wavelength 254nm, collection time 135-180min, the effluent was concentrated and dried to obtain Schisandra triterpene powder.
实施例2Example 2
北五味子藤茎1000g，先将原料切成1.5cm长度后放入高速组织匀浆捣碎机在12000rpm条件下保持15min后，按照液料比[溶剂体积(mL)/原料重量(g)]13mL∶1g加入浓度80％氯仿溶液13000mL后，再加入北五味子藤茎原料重量比为0.5％纤维素酶5g，在超声功率600W、40℃条件下，酶解20min后，再在75℃恒温干燥18h，粉碎过60目筛为粉末备用。Schisandra chinensis cane 1000g, first cut the raw material into 1.5cm length, put it into a high-speed tissue homogenizer and grinder, keep it for 15min under the condition of 12000rpm, according to the liquid-solid ratio [solvent volume (mL) / raw material weight (g)] 13mL : After adding 13000mL of 80% chloroform solution to 1g, then add Schisandra chinensis cane raw material weight ratio of 0.5% cellulase 5g, under the condition of ultrasonic power 600W, 40°C, after enzymolysis for 20min, then dry at 75°C for 18h , crushed through a 60-mesh sieve and used as powder for later use.
取过筛后粉末250g加入到超临界萃取釜中，设定萃取温度46℃、分离器温度55℃开始萃取加压，调节CO2流量恒定在18L/h，萃取釜压力恒定在18MPa后，启动夹带剂泵，按照液料比[溶剂体积(mL)/过筛后粉末重量(g)]为0.8mL∶1g、浓度为85％乙酸乙酯200mL和液料比为0.2mL∶1g、浓度为80％乙醇50mL组成的复合夹带剂混匀后，打入夹带剂釜，萃取135min后，收集北五味子萃取液，减压回收溶剂，真空干燥为干燥粉末备用。Take 250g of the sieved powder and put it into the supercritical extraction kettle, set the extraction temperature to 46°C and the temperature of the separator to 55°C to start the extraction and pressurize, adjust the CO2 flow to be constant at 18L/h, and the pressure of the extraction kettle to be constant at 18MPa, start Entrainer pump, according to the ratio of liquid to material [volume of solvent (mL)/weight of powder after sieving (g)] is 0.8mL: 1g, concentration is 85% ethyl acetate 200mL and ratio of liquid to material is 0.2mL: 1g, concentration is After mixing the composite entrainer composed of 50mL of 80% ethanol, put it into the entrainer tank, extract for 135min, collect the extract of Schisandra chinensis, recover the solvent under reduced pressure, and vacuum dry it as a dry powder for later use.
称取真空干燥后粉末10g，加入按照液料比[溶剂体积(mL)/真空干燥后粉末重量(g)]为10mL∶1g、浓度为80％正丙醇100mL，液料比为8mL∶1g、浓度为75％乙酸乙酯80mL，液料比为6mL∶1g、浓度为90％氯仿60mL，液料比为10mL∶1g纯净水(市场上提供的纯净水)100mL组成的复合溶剂中，在分液漏斗中平衡24h后，使用前分离成上相(固定相)和下相(流动相)，分别脱气后备用，取上下相配制成样品溶液，注入高速逆流色谱，选择转速为850r/min、流量为3.5mL/min、检测波长为254nm，收集时间135-180min，对流出液进行浓缩、干燥，制得北五味子三萜粉末。Weigh 10g of the powder after vacuum drying, add 10mL: 1g according to the liquid-material ratio [solvent volume (mL)/powder weight after vacuum drying (g)], the concentration is 80% n-propanol 100mL, the liquid-material ratio is 8mL: 1g , concentration is 75% ethyl acetate 80mL, liquid-to-material ratio is 6mL: 1g, concentration is 90% chloroform 60mL, liquid-to-solid ratio is 10mL: in the compound solvent that 1g pure water (purified water provided on the market) 100mL forms, in After equilibrating in the separatory funnel for 24 hours, separate into upper phase (stationary phase) and lower phase (mobile phase) before use, degas respectively and prepare for use. Take the upper and lower phases to prepare a sample solution, inject high-speed countercurrent chromatography, and select the rotation speed as 850r/ min, the flow rate is 3.5mL/min, the detection wavelength is 254nm, and the collection time is 135-180min. The effluent is concentrated and dried to obtain Schisandra triterpenoid powder.
实施例3Example 3
北五味子藤茎1000g，先将原料切成2cm长度后放入高速组织匀浆捣碎机在12000rpm条件下保持15min后，按照液料比[溶剂体积(mL)/原料重量(g)]13mL∶1g加入浓度80％氯仿溶液13000mL后，再加入北五味子藤茎原料重量比为0.5％纤维素酶5g，在超声功率600W、40℃条件下，酶解20min后，再在75℃恒温干燥18h，粉碎过60目筛为粉末备用。Schisandra chinensis cane 1000g, first cut the raw material into 2cm length and put it into a high-speed tissue homogenizer and grinder, keep it for 15min under the condition of 12000rpm, according to the ratio of liquid to material [volume of solvent (mL)/weight of raw material (g)] 13mL: After 1 g of 80% chloroform solution 13000mL was added, then 5 g of cellulase with a weight ratio of 0.5% of Schisandra chinensis cane raw material was added. Under the condition of ultrasonic power of 600W and 40°C, after enzymatic hydrolysis for 20min, it was then dried at a constant temperature of 75°C for 18h. Crushed through a 60-mesh sieve as powder for later use.
取过筛后粉末300g加入到超临界萃取釜中，设定萃取温度46℃、分离温度55℃开始萃取加压，调节CO2流量恒定在18L/h，萃取釜压力恒定在18MPa后，启动夹带剂泵，按照液料比[溶剂体积(mL)/过筛后粉末重量(g)]为0.8mL∶1g、浓度为85％乙酸乙酯240mL和液料比为0.2mL∶1g、浓度为80％乙醇60mL组成的复合夹带剂混匀后，打入夹带剂釜，萃取135min后，收集北五味子萃取液，减压回收溶剂，真空干燥为干燥粉末备用。Take 300g of the sieved powder and add it to the supercritical extraction kettle, set the extraction temperature to 46°C, and the separation temperature to 55°C to start extraction and pressurization, adjust the CO2 flow to be constant at 18L/h, and after the pressure of the extraction kettle is constant at 18MPa, start entrainment Agent pump, according to the ratio of liquid to material [volume of solvent (mL)/weight of powder after sieving (g)] is 0.8mL: 1g, concentration is 85% ethyl acetate 240mL and ratio of liquid to material is 0.2mL: 1g, concentration is 80 After mixing the compound entrainer composed of 60 mL of % ethanol, put it into the entrainer tank, extract for 135 minutes, collect the extract of Schisandra chinensis, recover the solvent under reduced pressure, and dry it in vacuum to obtain a dry powder for later use.
称取真空干燥后粉末10g，加入按照液料比[溶剂体积(mL)/真空干燥后粉末重量(g)]为10mL∶1g、浓度为80％正丙醇100mL，液料比为8mL∶1g、浓度为75％乙酸乙酯80mL，液料比为6mL∶1g、浓度为90％氯仿60mL，液料比为10mL∶1g纯净水100mL组成的复合溶剂中，在分液漏斗中平衡24h后，使用前分离成上相(固定相)和下相(流动相)，分别脱气后备用，取上下相配制成样品溶液，注入高速逆流色谱，选择转速850r/min，流量3.5mL/min，检测波长为254nm，收集时间135-180min，对流出液进行浓缩、干燥，制得北五味子三萜粉末。Weigh 10g of the powder after vacuum drying, add 10mL: 1g according to the liquid-material ratio [solvent volume (mL)/powder weight after vacuum drying (g)], the concentration is 80% n-propanol 100mL, the liquid-material ratio is 8mL: 1g , concentration is 75% ethyl acetate 80mL, liquid-to-solid ratio is 6mL: 1g, concentration is 90% chloroform 60mL, liquid-to-solid ratio is 10mL: in the compound solvent that 1g pure water 100mL forms, after equilibrating in separating funnel 24h, Before use, it is separated into upper phase (stationary phase) and lower phase (mobile phase), degassed respectively and then used for later use. The upper and lower phases are taken to prepare a sample solution, injected into high-speed countercurrent chromatography, and the rotation speed is selected to be 850r/min, and the flow rate is 3.5mL/min. The wavelength is 254nm, the collection time is 135-180min, and the effluent is concentrated and dried to obtain Schisandra triterpenoid powder.
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