WO2017177706A1 - 一种油茶果壳多糖的提取工艺 - Google Patents

一种油茶果壳多糖的提取工艺 Download PDF

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Publication number
WO2017177706A1
WO2017177706A1 PCT/CN2016/109825 CN2016109825W WO2017177706A1 WO 2017177706 A1 WO2017177706 A1 WO 2017177706A1 CN 2016109825 W CN2016109825 W CN 2016109825W WO 2017177706 A1 WO2017177706 A1 WO 2017177706A1
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extraction
camellia oleifera
microwave
camellia
ultrasonic
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PCT/CN2016/109825
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English (en)
French (fr)
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续旭
毕德成
张永夏
陈培锋
廖伟良
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深圳大学
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Publication of WO2017177706A1 publication Critical patent/WO2017177706A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass

Definitions

  • the invention belongs to the technical field of chemical industry, and particularly relates to a process for extracting polysaccharides from Camellia oleifera.
  • Camellia is the main woody oil in China, and it is also the world's four woody edible oils.
  • Camellia husk is the shell of camellia, which is the main by-product of the production of camellia and is rich in resources.
  • Camellia oleifera is an abandonment resource.
  • Camellia oleracea polysaccharide extracted from Camellia oleifera has biological activities such as anti-tumor, anti-oxidation and blood lipid-lowering effects. It has been used in food, environmental protection, beauty care and other days. It has been used in the chemical industry, especially in the field of biomedicine.
  • the technical problem to be solved by the present invention is to overcome the defects of the prior art and provide an extraction process of Camellia oleifera polysaccharide.
  • the present invention is achieved by the method for extracting Camellia oleracea polysaccharide, which comprises the following steps:
  • the Camellia husk powder is passed through a 40-60 mesh sieve to obtain a treated powder
  • the mixture is subjected to ultrasonic and/or microwave extraction, wherein the ultrasonic extraction conditions are: ultrasonic extraction at 85-100 ° C 15-35 Min, the microwave extraction condition is: maintaining 5 ⁇ 9 under microwave of 240-700 W Min, the extract is concentrated at 40-50 ° C and then added to ethanol, wherein the volume fraction of ethanol reaches 80% or more, and then the alcohol is precipitated at 3 to 5 ° C for more than 12 hours, and the precipitate is separated to obtain the camellia polysaccharide.
  • the ultrasonic extraction conditions are: ultrasonic extraction at 85-100 ° C 15-35 Min
  • the microwave extraction condition is: maintaining 5 ⁇ 9 under microwave of 240-700 W Min
  • the extract is concentrated at 40-50 ° C and then added to ethanol, wherein the volume fraction of ethanol reaches 80% or more, and then the alcohol is precipitated at 3 to 5 ° C for more than 12 hours, and the precipitate is separated to obtain the camellia polysaccharide.
  • the invention provides a process for extracting the oil of tea husk, which uses the oil tea husk as a raw material, the extraction rate of the tea husk polysaccharide and the uronic acid content are comparative parameters, and the uronic acid content is determined by the phenol sulfuric acid method, which proves ultrasonic extraction. And/or microwave extraction and traditional water extraction have obvious advantages for Camellia oleifera polysaccharides.
  • the extraction process is simple and easy, the extraction rate is high, and the cost is low, which is beneficial to industrial applications.
  • FIG. 1 is a graph showing the effect of ultrasonic extraction time on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 2 is a graph showing the effect of ultrasonic extraction time on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 3 is a graph showing the effect of different extraction times of ultrasonic extraction on the uronic acid content of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 4 is a diagram showing the effect of ultrasonic extraction time on the content of uronic acid of Camellia oleifera in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 5 is a graph showing the effect of microwave time on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 6 is a graph showing the effect of microwave extraction time on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 7 is a diagram showing the effect of microwave time on the content of uronic acid of Camellia oleifera in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 8 is a graph showing the effect of microwave extraction time on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • FIG. 9 is a graph showing the effect of microwave power on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention.
  • Figure 10 is a graph showing the effect of microwave extraction power on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • Figure 11 is a graph showing the effect of microwave power on the content of uronic acid of Camellia oleifera in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • Figure 12 is a graph showing the effect of microwave extraction power on the extraction rate of Camellia oleifera polysaccharides in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • Figure 13 is a graph showing the extraction rate of Camellia oleifera polysaccharides in a comprehensive experiment of the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • Figure 14 is a diagram showing the results of a comprehensive experiment of the content of uronic acid of Camellia oleifera in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • 15 is a diagram showing the results of synergistic extraction by ultrasonic method and microwave method in the extraction process of Camellia oleifera polysaccharides according to an embodiment of the present invention
  • Figure 16 is a graph showing the results of an aqueous extraction experiment provided in Comparative Example 1 of the present invention.
  • the embodiment of the invention provides a process for extracting Camellia oleracea polysaccharide, which comprises the following steps:
  • the ultrasonic extraction conditions are: ultrasonic extraction at 85-100 ° C 15-35 Min
  • the microwave extraction condition is: maintaining 5 ⁇ 9 under microwave of 240-700 W Min
  • the extract is concentrated at 40-50 ° C and then added to ethanol, wherein the volume fraction of ethanol reaches 80% or more, and then the alcohol is precipitated at 3 to 5 ° C for more than 12 hours, and the precipitate is separated to obtain the camellia polysaccharide.
  • step S01 the oil tea husk powder is passed through a 40-60 mesh sieve to increase the extraction rate.
  • step S02 the mass ratio of the camellia nut shell powder to water is preferably from 1:14 to 16.
  • step S03 the ultrasonic extraction and microwave extraction may be repeated, for example, ultrasonic extraction twice, or microwave extraction twice, or microwave extraction after ultrasonic extraction, or ultrasonic extraction after microwave extraction.
  • the extract is separated, and step S02 is repeated for the next extraction.
  • the ultrasonic extraction is specifically: ultrasonically extracting the mixture at a constant temperature of 80 to 100 ° C in an ultrasonic apparatus, and ultrasonic extraction may be repeated 1 to 3 times, and after each ultrasonic extraction, the extraction liquid is separated, and then step S02 is repeated, exceeding In the case of 2 extractions, the extracts were combined, and the extract was concentrated in a vacuum at 40-50 ° C. A certain volume of absolute ethanol was added to make the ethanol volume fraction of the extract reach 80%, and the alcohol was precipitated at 3 to 5 °C.
  • the precipitate and the supernatant are separated after the alcohol precipitation, wherein the separation may be carried out by centrifugation, and the precipitate may be dissolved in an appropriate amount of ultrapure water, and freeze-dried under vacuum to obtain Camellia oleifera polysaccharide. Further, preferably, the mixture is sonicated at 85 to 95 °C.
  • Ultrasonic extraction time has a certain effect on the extraction rate of Camellia oleifera polysaccharides.
  • Figure 1 shows the effect of ultrasonic extraction time on the extraction rate of Camellia oleifera polysaccharides.
  • Figure 2 is the effect of ultrasonic extraction time on the extraction rate of Camellia oleifera polysaccharides. It can be seen from Fig. 1 and Fig. 2 that the longer the extraction time, the higher the extraction rate of the oil tea husk polysaccharide, and the data deviation of each group in the parallel experiment is within a reasonable error range. When the time was less than 30 min, the extraction rate of Camellia oleifera polysaccharides increased rapidly.
  • the extraction rate of Camellia oleracea polysaccharides grew slowly.
  • the extraction time of Camellia oleifera polysaccharides was positively correlated with the extraction rate.
  • the time had a great influence on the extraction rate of Camellia oleifera polysaccharides.
  • the extraction rate of Camellia oleifera polysaccharides was affected.
  • the extraction time has less impact. Therefore, preferably, the time for ultrasonic extraction is 25 to 35 Min.
  • Fig. 3 is the effect of different extraction time of ultrasonic extraction on the content of uronic acid of Camellia oleifera.
  • Fig. 4 is the effect of ultrasonic extraction time on the content of uronic acid of Camellia oleifera. It can be seen from Fig. 3 and Fig. 4 that under the action of ultrasonic waves, when the extraction time is less than 30 min, the content of uronic acid in the oil tea of each group is higher than that of the water extraction method and its sugar The content of aldonic acid was in increasing relationship with the extraction time. After the extraction time exceeded 30 min, the content of uronic acid in the tea group of the experimental group was lower than that of the water extraction method.
  • the time of the ultrasonic extraction is 25 to 35 min.
  • the microwave extraction is specifically: the mixture is placed in a microwave environment for extraction, such as in a microwave oven, at 240-700 Maintain 5 to 9 under microwave Min.
  • the microwave extraction can be repeated 1 or 3 times.
  • the extract is separated, and step S02 is repeated.
  • the extract is combined in more than 2 extractions, and all the extracts are concentrated in a vacuum at 40-50 ° C to a viscous state. Adding a certain volume of absolute ethanol to make the volume fraction of ethanol in the extract reach 80%, and alcohol precipitation at 3 to 5 °C for more than 12 hours. After the alcohol precipitation, the precipitate and the supernatant are centrifuged, and the precipitate can be used with an appropriate amount of ultrapure water. Dissolved, vacuum freeze-dried to obtain Camellia oleracea polysaccharide.
  • Figure 5 is the effect of microwave time on the extraction rate of Camellia oleifera polysaccharides
  • Figure 6 is the effect of microwave extraction time on the extraction rate of Camellia oleifera polysaccharides.
  • the extraction power is 540W
  • the solid-liquid mass ratio of Camellia oleifera powder to water is 1:15
  • the volume fraction of alcohol ethanol is 80%
  • the extraction time is 2
  • the extraction rate of Camellia oleifera polysaccharides is different. affect the result.
  • the average value of the experimental data obtained from the three parallel experiments was used as the result data of the experiment, and the standard error between the three sets of parallel data was calculated.
  • Figure 7 is the effect of microwave time on the content of uronic acid in Camellia oleifera
  • Figure 8 is the effect of microwave extraction time on the extraction rate of Camellia oleifera.
  • the result is a change in the uronic acid content of the extracted Camellia oleifera polysaccharide under the conditions. It can be seen from Fig. 7 and Fig. 8 that under the microwave method, the uronic acid content of Camellia oleifera polysaccharide is obviously increased, but when the extraction time is 11 min, the uronic acid content of Camellia oleifera polysaccharide is low and higher than that of water extraction.
  • the extracted tea camellia polysaccharide has a low content of uronic acid.
  • Figure 9 shows the effect of microwave power on the extraction rate of Camellia oleifera polysaccharides
  • Figure 10 shows the effect of microwave extraction power on the extraction rate of Camellia oleifera polysaccharides.
  • the microwave extraction condition was 5 min extraction time, the solid-liquid mass ratio of the oil tea shell powder to water was 1:15, the alcohol precipitation ethanol volume fraction was 80%, and the extraction frequency was 2.
  • the average value of the experimental data obtained from the three parallel experiments was used as the result data of the experiment, and the standard error between the three sets of parallel data was calculated.
  • Figure 11 shows the effect of microwave power on the content of uronic acid in Camellia oleifera
  • Figure 12 shows the effect of microwave extraction power on the extraction rate of Camellia oleifera. It can be seen from Fig. 11 and Fig. 12 that the content of uronic acid in the microwave-derived Camellia oleifera polysaccharide is slightly lower than that in the extract of Camellia oleifera. Before the extraction power was 540W, the uronic acid content of Camellia oleifera polysaccharide increased with the increase of power, and the uronic acid content increased faster between 380W and 540W.
  • the microwave power factor should take power of 240W, 380W and 540W, and the microwave time factor should take time points of 5min, 7min and 9min.
  • Figure 13 is a graph showing the extraction rate of Camellia oleifera polysaccharides in a comprehensive experiment. From the experimental data of Fig. 13, it can be known that the order of the conditions affecting the extraction rate of the oil tea husk polysaccharide is: A3B2>A2B3>A3B3>A2B1>A3B1>A1B3>A1B1>A1B2>A2B2. Therefore, the best combination of microwave method affecting the extraction rate of Camellia oleifera polysaccharides is A3B2.
  • Figure 14 is a result of the uronic acid content of Camellia oleifera in a comprehensive experiment. From the experimental data of Fig. 14, it can be known that the order of the conditions affecting the size of the uronic acid content of Camellia oleifera is: A3B2>A3B3>A3B1>A1B3>A2B3>A2B2>A1B1>A1B2>A2B1. Therefore, the best combination of microwave method affecting the content of uronic acid in Camellia oleifera is A3B2.
  • the preferred process conditions of the microwave method are extraction power of 540W, extraction time of 7min, solid-liquid mass ratio of Camellia husk powder to water is 1:15, and alcoholic ethanol volume fraction is 80. %, the number of extractions is 2.
  • the extraction rate of Camellia oleifera polysaccharide was 9.6%
  • the uronic acid content was 36.41%.
  • ultrasonic extraction and microwave extraction were used to extract the experimental conditions under the above-mentioned research.
  • the optimal process conditions of ultrasonic extraction and the preferred process conditions of microwave extraction were used to assist the extraction of Camellia oleifera polysaccharides.
  • Synergistic extraction can improve the extraction effect of Camellia oleifera polysaccharides.
  • the Camellia oleifera powder was passed through a 50 mesh sieve and mixed with water.
  • the solid-liquid mass ratio of Camellia husk powder to water was 1:15, and a mixture was obtained, and the mixture was ultrasonically extracted at 90 ° C. Min, extracted twice, the two extracts were mixed, and the extract was concentrated in a vacuum at 40-50 ° C to a viscous state.
  • a certain volume of absolute ethanol was added to make the ethanol volume fraction of the extract reach 80%, and the alcohol was at 3 to 5 ° C.
  • the Camellia oleifera powder was passed through a 50 mesh sieve and mixed with water.
  • the solid-liquid mass ratio of Camellia husk powder to water was 1:15, and the mixture was obtained.
  • the mixture was placed in a microwave oven, extracted at 540 W for 7 min, extracted twice, two
  • the secondary extract is mixed, and the extract is concentrated in a vacuum at 40-50 ° C, and a certain volume of absolute ethanol is added to make the volume fraction of ethanol in the extract reach 80%, and the alcohol is precipitated at 3 to 5 ° C for 24 hours.
  • the precipitate and the supernatant were separated by centrifugation, and the precipitate was dissolved in an appropriate amount of ultrapure water, and freeze-dried under vacuum to obtain a crude polysaccharide of Camellia oleifera.
  • a certain amount of polysaccharide extract was weighed, and the uronic acid content was determined by a phenol sulfuric acid method.
  • the extraction rate of Camellia oleifera polysaccharide was 9.6%, and the uronic acid content was 36.41%.
  • the Camellia oleifera powder was passed through a 50 mesh sieve and mixed with water.
  • the solid-liquid mass ratio of Camellia husk powder to water was 1:15, and a mixture was obtained, and the mixture was ultrasonically extracted at 90 ° C. Min, 540W extraction for 7min, extraction twice, two extracts mixed, 40 ⁇ 50 ° C vacuum concentrated extract to a viscous, adding a volume of absolute ethanol to make the ethanol volume fraction of the extract reached 80%, in 3 ⁇
  • the alcohol was precipitated at 5 ° C for 24 hours.
  • Camellia husk powder is passed through a 50 mesh sieve and extracted in hot water at 90 ° C. Min, the solid-liquid mass ratio of Camellia oleifera powder to water is 1:15. After extracting twice, the extract is combined, and the extract is concentrated in vacuo to a viscous state at 45 ° C. A certain volume of absolute ethanol is added to make the ethanol volume in the extract. The score reached 80%, and the alcohol was precipitated in a refrigerator at 4 ° C for 24 hours. After the alcohol precipitation, the precipitate and the supernatant were centrifuged, and the precipitate was dissolved in an appropriate amount of ultrapure water, and vacuum-dried to obtain a crude polysaccharide of Camellia oleifera. A certain amount of polysaccharide extract was weighed, and the uronic acid content was determined by a phenol sulfuric acid method.

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Abstract

本发明涉及一种油茶果壳多糖的提取工艺，其包括如下步骤：将油茶果壳粉末过40～60目筛，得处理粉末；将所述处理粉末与水混合，其中，油茶果壳粉末和水的质量比为1：10～20，得混合物；将所述混合物进行超声和／或微波提取，其中，所述超声提取的条件为：在80～100℃超声提取15～35 min，所述微波提取的条件为：在240～700 W的微波下保持5～9 min；提取液在40～50℃浓缩后加入乙醇，其中，乙醇体积分数达到80%以上，然后在3～5℃醇沉12小时以上，分离沉淀物，获得所述油茶果壳多糖。该提取工艺简单易行，提取率高，成本低，有利于工业化应用。

Description

一种油茶果壳多糖的提取工艺 技术领域
本发明属于化工技术领域，具体涉及一种油茶果壳多糖的提取工艺。
背景技术
油茶是我国主要木本油料，也是世界四大木本食用油料。油茶果壳是油茶果外壳，是油茶生产的主要副产品，资源丰富。油茶果壳是一种废弃资源，据文献报告，从油茶果壳中提取的油茶果壳多糖具有抗肿瘤、抗氧化、降血脂作用等生物学活性，已经在食品、环保、美容保健和其它日用化学工业有所应用，特别是在生物医药领域日益受到关注。然而目前，油茶果壳大多被农民直接燃烧，少数作为工业资源利用但方法单一，如制备活性炭或提取抗氧化物质或提取多糖或提取茶皂素等，很少综合利用。因此，有必要开发一种综合利用油茶果壳资源制备高附加值产品的方法。
技术问题
本发明所要解决的技术问题在于克服现有技术的缺陷，提供一种油茶果壳多糖的提取工艺。
技术解决方案
本发明是这样实现的，一种油茶果壳多糖的提取工艺，其包括如下步骤：
将油茶果壳粉末过40～60目筛，得处理粉末；
将所述处理粉末与水混合，其中，油茶果壳粉末和水的质量比为1：10～20，得混合物；
将所述混合物进行超声和／或微波提取，其中，所述超声提取的条件为：在80～100℃超声提取15～35 min，所述微波提取的条件为：在240～700 W的微波下保持5～9 min，提取液在40～50℃浓缩后加入乙醇，其中，乙醇体积分数达到80%以上，然后在3～5℃醇沉12小时以上，分离沉淀物，获得所述油茶果壳多糖。
 有益效果
本发明提供一种油茶果壳多糖的提取工艺，其以油茶果壳为原料，油茶果壳多糖的提取率和糖醛酸含量为比较参数，采用苯酚硫酸法测定糖醛酸含量，证明超声提取和／或微波提取与传统水提法对油茶果壳多糖均有明显的优势。该提取工艺简单易行，提取率高，成本低，有利于工业化应用。
附图说明
图1是本发明实施例油茶果壳多糖的提取工艺中超声提取时间对油茶果壳多糖提取率的影响结果图；
图2是本发明实施例油茶果壳多糖的提取工艺中超声提取时间对油茶果壳多糖提取率的影响图；
图3是本发明实施例油茶果壳多糖的提取工艺中超声提取之不同提取时间对油茶果壳多糖糖醛酸含量影响结果图；
图4是本发明实施例油茶果壳多糖的提取工艺中超声提取时间对油茶果壳多糖糖醛酸含量的影响图；
图5是本发明实施例油茶果壳多糖的提取工艺中微波时间对油茶果壳多糖提取率的影响结果图；
图6是本发明实施例油茶果壳多糖的提取工艺中微波提取时间对油茶果壳多糖提取率的影响图；
图7是本发明实施例油茶果壳多糖的提取工艺中微波时间对油茶果壳多糖糖醛酸含量的影响图；
图8是本发明实施例油茶果壳多糖的提取工艺中微波提取时间对油茶果壳多糖提取率的影响图；
图9为本发明实施例油茶果壳多糖的提取工艺中微波功率对油茶果壳多糖提取率的影响结果图；
图10是本发明实施例油茶果壳多糖的提取工艺中微波提取功率对油茶果壳多糖提取率的影响图；
图11是本发明实施例油茶果壳多糖的提取工艺中微波功率对油茶果壳多糖糖醛酸含量的影响结果图；
图12是本发明实施例油茶果壳多糖的提取工艺中微波提取功率对油茶果壳多糖提取率的影响图；
图13是本发明实施例油茶果壳多糖的提取工艺中全面实验之油茶果壳多糖提取率结果图；
图14是本发明实施例油茶果壳多糖的提取工艺中全面实验之油茶果壳多糖糖醛酸含量结果图；
图15是本发明实施例油茶果壳多糖的提取工艺中超声波法和微波法协同提取结果图；
图16是本发明对比例1提供的水提法实验结果图。
 本发明的实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及具体实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
本发明实施例提供一种油茶果壳多糖的提取工艺，其包括如下步骤：
S01：将油茶果壳粉末过40～60目筛，得处理粉末；
S02：将所述处理粉末与水混合，其中，油茶果壳粉末和水的质量比为1：10～20，得混合物；
S03：将所述混合物进行超声和／或微波提取，其中，所述超声提取的条件为：在80～100℃超声提取15～35 min，所述微波提取的条件为：在240～700 W的微波下保持5～9 min，提取液在40～50℃浓缩后加入乙醇，其中，乙醇体积分数达到80%以上，然后在3～5℃醇沉12小时以上，分离沉淀物，获得所述油茶果壳多糖。
步骤S01中，油茶果壳粉末过40～60目筛，以提高提取率。
步骤S02中，所述油茶果壳粉末和水的质量比优选为1：14～16。
步骤S03中，所述超声提取和微波提取可以重复，例如超声提取两次，或者微波提取两次，又或者超声提取后微波提取，或者微波提取后超声提取。每次提取后，分离出提取液，再重复步骤S02进行下一次提取。
所述超声提取具体为：将所述混合物在80～100℃恒温在超声波仪中超声提取，超声提取可以重复1～3次，每次超声提取后，分离出提取液，再重复步骤S02，超过2次提取的情况下合并提取液，40～50℃真空浓缩提取液至粘稠状，加入一定体积的无水乙醇使提取液中乙醇体积分数达到80%，在3～5℃下醇沉12小时以上，醇沉后分离沉淀物与上清液，其中，所述分离可选用离心，沉淀物可以用适量超纯水溶解，真空冷冻干燥得到油茶果壳多糖。进一步，优选地，所述混合物在85～95℃下超声。
超声提取时间对油茶果壳多糖提取率具有一定的影响。图1是超声提取时间对油茶果壳多糖提取率的影响结果，图2是超声提取时间对油茶果壳多糖提取率的影响图。由图1和图2可以看出，提取时间越长，油茶果壳多糖提取率越高，且平行实验中各组数据偏差在合理误差范围内。时间低于30min时，油茶果壳多糖提取率增长趋势较快，高于30min后，油茶果壳多糖提取率增长趋势较慢。结合数据分析可知，油茶果壳多糖提取时间与提取率成正相关，提取时间低于30min时，时间对油茶果壳多糖提取率影响较大，提取时间高于30min后，油茶果壳多糖提取率受提取时间影响较小。因此，优选地，超声提取的时间为25～35 min。
图3是超声提取之不同提取时间对油茶果壳多糖糖醛酸含量影响结果，图4是超声提取时间对油茶果壳多糖糖醛酸含量的影响图。由图3和图4可以看出，在超声波的作用下，提取时间低于30min时，每组实验组的油茶果壳多糖糖醛酸含量均高于水提法的糖醛酸含量且其糖醛酸含量与提取时间成递增关系，提取时间超过30min后，实验组的油茶果壳多糖糖醛酸含量均低于水提法的糖醛酸含量。
因此，优选地，所述超声提取的时间为25～35 min。
所述微波提取具体为：将所述混合物置于微波环境下进行提取，如微波炉中，在240～700 W的微波下保持5～9 min。微波提取可以重复1～3次，每次微波提取后，分离出提取液，再重复步骤S02，超过2次提取的情况下合并提取液，40～50℃真空浓缩所有提取液至粘稠状，加入一定体积的无水乙醇使提取液中乙醇体积分数达到80%，在3～5℃下醇沉12小时以上，醇沉后离心分离沉淀物与上清液，沉淀物可以用适量超纯水溶解，真空冷冻干燥得到油茶果壳多糖。
图5是微波时间对油茶果壳多糖提取率的影响结果，图6是微波提取时间对油茶果壳多糖提取率的影响图。其为提取功率为540W，油茶果壳粉末与水的固液质量比为1：15，醇沉乙醇体积分数为80%，提取次数为2的情况下不同提取时间对油茶果壳多糖提取率的影响结果。以三组平行实验所获得实验数据的平均数值作为本实验的结果数据，并且计算三组平行数据之间的标准误差。
由图5和图6得知，在微波法条件下，油茶果壳多糖的提取率很明显地提高，在提取时间为7min之前，油茶果壳多糖的提取率随时间的增加而升高，5min至7min之间提取率增长趋势更快；当提取时间超过7min，油茶果壳多糖的提取率随时间的增加而降低。当提取时间为7min时，油茶果壳多糖的提取率最高，且平行实验中各组数据偏差在合理误差范围内。
图7是微波时间对油茶果壳多糖糖醛酸含量的影响结果，图8为微波提取时间对油茶果壳多糖提取率的影响图。结果为该条件下所提取的油茶果壳多糖中糖醛酸含量变化。由图7和图8得知，在微波法条件下，油茶果壳多糖的糖醛酸含量很明显地提高，但提取时间为11min时，油茶果壳多糖的糖醛酸含量低且比水提法提取的油茶果壳多糖糖醛酸含量低。在提取时间为7min之前，油茶果壳多糖的糖醛酸含量随时间的增加而升高，5min至7min之间糖醛酸含增长趋势更快；当提取时间超过7min，油茶果壳多糖的糖醛酸含随时间的增加而降低。当提取时间为7min时，油茶果壳多糖的糖醛酸含最高。
图9为微波功率对油茶果壳多糖提取率的影响结果，图10为微波提取功率对油茶果壳多糖提取率的影响图。其微波提取的条件为提取时间5min，油茶果壳粉末与水的固液质量比为1：15，醇沉乙醇体积分数为80%，提取次数为2。以三组平行实验所获得实验数据的平均数值作为本实验的结果数据，并且计算三组平行数据之间的标准误差。
由图9和图10得知，在微波法条件下，油茶果壳多糖的提取率很明显地提高，在提取功率为540W之前，油茶果壳多糖的提取率随时间的增加而升高；当提取攻率超过540W，油茶果壳多糖的提取率随时间的增加而降低。当提取功率为540W时，油茶果壳多糖的提取率最高，平行实验中各组数据偏差在合理误差范围内，且每组实验组油茶果壳多糖提取率均高于水提法的油茶果壳多糖提取率。
图11为微波功率对油茶果壳多糖糖醛酸含量的影响结果，图12为微波提取功率对油茶果壳多糖提取率的影响图。由图11和图12得知，微波提取油茶果壳多糖的糖醛酸含量比水提法提取的油茶果壳多糖糖醛酸含量略低。在提取功率为540W之前，油茶果壳多糖的糖醛酸含量随功率的增加而升高，380W至540W之间糖醛酸含增长趋势更快；当提取功率超过540W，油茶果壳多糖的糖醛酸含随功率的增加而降低。当提取功率为540 W时，油茶果壳多糖的糖醛酸含最高。
综上所述，在后续全面实验中，微波功率因素应取功率为240W、380W和540W，微波时间因素应取时间点为5min、7min和9min。
对微波时间、微波功率全面实验研究。在单因素实验的基础上，全面实验设计为：提取功率、提取时间两个因素的综合影响，其中提取时间、提取功率各有3个水平。实验设A1、A2、A3分别对应240W、380W、540W，B1、B2、B3分别对应5min、7min、9min。以油茶果壳多糖提取率和糖醛酸含量为比较指标，筛选油茶果壳多糖微波法的最佳工艺条件。
图13是全面实验之油茶果壳多糖提取率结果。由图13实验结果数据可得知，影响油茶果壳多糖提取率的大小的条件组合顺序为：A3B2＞A2B3＞A3B3＞A2B1＞A3B1＞A1B3＞A1B1＞A1B2＞A2B2。所以微波法影响油茶果壳多糖提取率的最佳组合为A3B2。
图14为全面实验之油茶果壳多糖糖醛酸含量结果。由图14实验结果数据可得知，影响油茶果壳多糖糖醛酸含量的大小的条件组合顺序为：A3B2＞A3B3＞A3B1＞A1B3＞A2B3＞A2B2＞A1B1＞A1B2＞A2B1。所以微波法影响油茶果壳多糖糖醛酸含量的最佳组合为A3B2。
综上所述，从全面实验中，微波法的优选工艺条件为提取功率为540W，提取时间为7min，油茶果壳粉末与水的固液质量比为1：15，醇沉乙醇体积分数为80%，提取次数为2。在此实验条件下，油茶果壳多糖的提取率为9.6%，糖醛酸含量为36.41%。
同时选用超声提取和微波提取，提取根据上述研究所得实验条件，利用超声提取的优选工艺条件及微波提取的优选工艺条件协同辅助提取油茶果壳多糖，实验得出此条件下的油茶果壳多糖的多糖提取率和糖醛酸含量。协同提取能够提高油茶果壳多糖的提取效果。
由图15实验结果数据可得知，此条件下油茶果壳多糖的提取率为9.96%，糖醛酸含量为35.18%。超声提取和微波提取在最佳的条件下的提取效果均比水提法好，同微波提取的效果比超声提取的效果更明显。利用两种方法协同提取，效果显著提高。
以下结合具体实施例对本发明的具体实现进行详细描述。
实施例1：
油茶果壳粉末过50目筛，与水混合，油茶果壳粉末与水的固液质量比为1：15，得混合物，将所述混合物在90℃下超声提取30 min，提取两次，两次提取液混合，40～50℃真空浓缩提取液至粘稠状，加入一定体积的无水乙醇使提取液中乙醇体积分数达到80%，在3～5℃下醇沉24小时，醇沉后离心分离沉淀物与上清液，沉淀物用适量超纯水溶解，真空冷冻干燥得到油茶果壳粗多糖。称取一定量多糖提取物，用苯酚硫酸法测定其中糖醛酸含量。油茶果壳多糖提取率为5.63%，糖醛酸含量为29.47%。
实施例2：
油茶果壳粉末过50目筛，与水混合，油茶果壳粉末与水的固液质量比为1：15，得混合物，将所述混合物置于微波炉中，540W提取7min，提取两次，两次提取液混合，40～50℃真空浓缩提取液至粘稠状，加入一定体积的无水乙醇使提取液中乙醇体积分数达到80%，在3～5℃下醇沉24小时，醇沉后离心分离沉淀物与上清液，沉淀物用适量超纯水溶解，真空冷冻干燥得到油茶果壳粗多糖。称取一定量多糖提取物，用苯酚硫酸法测定其中糖醛酸含量。油茶果壳多糖的提取率为9.6%，糖醛酸含量为36.41%。
实施例3：
油茶果壳粉末过50目筛，与水混合，油茶果壳粉末与水的固液质量比为1：15，得混合物，将所述混合物在90℃下超声提取30 min，540W提取7min，提取两次，两次提取液混合，40～50℃真空浓缩提取液至粘稠状，加入一定体积的无水乙醇使提取液中乙醇体积分数达到80%，在3～5℃下醇沉24小时，醇沉后离心分离沉淀物与上清液，沉淀物用适量超纯水溶解，真空冷冻干燥得到油茶果壳粗多糖。称取一定量多糖提取物，用苯酚硫酸法测定其中糖醛酸含量。油茶果壳多糖的提取率为9.96%，糖醛酸含量为35.18%。
对比例1：
水提法
油茶果壳粉末过50目筛，在90℃热水中提取60 min，油茶果壳粉末与水的固液质量比为1：15，提取两次后合并提取液，45℃真空浓缩提取液至粘稠状，加入一定体积的无水乙醇使提取液中乙醇体积分数达到80%，在4℃冰箱冷藏醇沉24小时，醇沉后离心分离沉淀物与上清液，沉淀物用适量超纯水溶解，真空冷冻干燥得到油茶果壳粗多糖。称取一定量多糖提取物，用苯酚硫酸法测定其中糖醛酸含量。
由图16数据得知，油茶果壳多糖提取率的三组平行数据的平均数值为6.56%，糖醛酸含量三组平行数据的平均数值为28.91%，且平行实验中各组数据偏差在合理误差范围内。在此实验条件下，油茶果壳多糖提取率为6.56%，糖醛酸含量为28.91%。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种油茶果壳多糖的提取工艺，其特征在于，包括如下步骤：
    将油茶果壳粉末过40～60目筛，得处理粉末；
    将所述处理粉末与水混合，其中，油茶果壳粉末和水的质量比为1：10～20，得混合物；
    将所述混合物进行超声和／或微波提取，其中，所述超声提取的条件为：在80～100℃超声提取15～35 min，所述微波提取的条件为：在240～700 W的微波下保持5～9 min，提取液在40～50℃浓缩后加入乙醇，其中，乙醇体积分数达到80%以上，然后在3～5℃醇沉12小时以上，分离沉淀物，获得所述油茶果壳多糖。
  2. 如权利要求1所述的油茶果壳多糖的提取工艺，其特征在于，所述油茶果壳粉末和水的质量比为1：14～16。
  3. 如权利要求1所述的油茶果壳多糖的提取工艺，其特征在于，所述超声提取的条件为：在90～100℃下超声提取25～35 min。
  4. 如权利要求1或3所述的油茶果壳多糖的提取工艺，其特征在于，所述超声提取的条件为：在85～95℃超声提取25～35 min。
  5. 如权利要求1所述的油茶果壳多糖的提取工艺，其特征在于，所述微波提取的条件为：在240～700 W的微波下保持7 min。
  6. 如权利要求1或5所述的油茶果壳多糖的提取工艺，其特征在于，所述微波提取的条件为：在540W的微波下保持7 min。
  7. 如权利要求1所述的油茶果壳多糖的提取工艺，其特征在于，所述微波提取和／或超声提取的次数为1～3次，每次提取后，分离出提取液，再加入油茶果壳粉末10～20倍质量的水进行下一次提取。
  8. 如权利要求1所述的油茶果壳多糖的提取工艺，其特征在于，将所述混合物进行超声和微波提取。
  9. 如权利要求1或8所述的油茶果壳多糖的提取工艺，其特征在于，将所述混合物进行超声和微波提取，所述超声提取的条件为：在85～95℃超声提取25～35 min，所述微波提取的条件为：在540W的微波下保持7 min。
  10. 如权利要求1所述的油茶果壳多糖的提取工艺，其特征在于，所述分离沉淀物用离心的方法，所述分离后的沉淀物加水溶解后再进行冷冻干燥。
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CN113584204B (zh) * 2021-07-23 2023-06-23 中国林业科学研究院亚热带林业研究所 与油茶种子出仁率相关的dna片段、其紧密连锁的snp分子标记及其应用

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