CN101268815A - Supercritical carbonic anhydride wall-breaking method for melissa powder - Google Patents

Supercritical carbonic anhydride wall-breaking method for melissa powder Download PDF

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CN101268815A
CN101268815A CN 200810007855 CN200810007855A CN101268815A CN 101268815 A CN101268815 A CN 101268815A CN 200810007855 CN200810007855 CN 200810007855 CN 200810007855 A CN200810007855 A CN 200810007855A CN 101268815 A CN101268815 A CN 101268815A
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pollen
broken
carbon dioxide
bee pollen
bee
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CN 200810007855
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CN101268815B (en
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孙丽萍
张智武
响 徐
高彦祥
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中国农业科学院蜜蜂研究所
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Abstract

The invention discloses a method using supercritical carbon dioxide to perform bee pollen broken-face. Bee pollen is put in an extraction plant of supercritical carbon dioxide, to react for a certain time in supercritical carbon dioxide liquid at the proper pressure and temperature, a vent valve is opened to rapidly empty carbon dioxide, so that a pollen cell expands acutely due to larger pressure difference of the inside and the outside, thereby cracking. The method has the advantages that the operation is simple and convenient, the cost is low, the whole process is performed below 50 DEG C, the broken-face time does not exceed 30 minutes, the influence of the product by thermotropy is reduced, so that the active ingredient is preserved completely, at the same time, bacillus can be killed, the unification of the broken-face and the sterilization processes is realized, the broken-face ratio of the pollen cell is high, but the percentage of damage is low, and the inclusion still exists in a cracked pollen wall under the dry condition, thereby favoring the preservation of the nutritious content.

Description

蜂花粉超临界二氧化碳破壁方法技术领域本发明属于天然产物保健品和制药技术领域,涉及蜂花粉破壁方法,可以广泛应用在生物制药、保健食品等行业中。 Bee Pollen TECHNICAL FIELD The present invention is supercritical carbon dioxide are natural health products and pharmaceutical products relates to the field Bee Pollen method can be widely used in pharmaceuticals, health food and other industries. 背景技术蜂花粉是由蜜蜂采集蜜粉源植物的花粉经加工而形成的团状物,蜂花粉的营养成分十分丰富,几乎含有全部营养素,是一种高质量的营养源,不仅含有丰富的蛋白质、糖类、脂类、维生素、有机酸、矿物质、核酸,还含有酶和其他生物活性物质,被誉为"微型营养库"。 BACKGROUND OF THE INVENTION Bee pollen is collected by the bee pollen foraging plants dough formed by machining, bee pollen is nutrient rich, containing almost all the nutrients, a nutrient source is a high quality, not only rich in protein , carbohydrates, lipids, vitamins, organic acids, minerals, nucleic acids, also contains enzymes and other biologically active substances, known as "micro-nutrition library." 数千年前,在中国和希腊等古国,人们已开始食用花粉,并将其作为药用。 Thousands of years ago, in ancient China and Greece, people have begun to eat pollen, and as a medicinal. 随着科学技术的发展和研究的深入,蜂花粉的医疗保健功能被逐步发掘,如防治心血管疾病、前列腺疾病、高血压、贫血、糖尿病等。 With the development of science and technology and research, bee pollen health care functions are gradually explore, such as the prevention and treatment of cardiovascular disease, prostate disease, high blood pressure, anemia, diabetes and so on. 人们己经不满足于食用蜂花粉所带来的缓慢的保健作用,从蜂花粉中提取功能明确的活性成分已成热潮,而有效提取活性成分的前提是进行蜂花粉的破壁。 People have not satisfied with the slow consumption of bee pollen health effects brought about by the extraction of active ingredients has become clear functional boom from bee pollen, and effective extraction of active ingredients is the premise of bee pollen broken. 目前国内外报道的花粉破壁方法有以下几种:(1) 温差破壁法(专利申请号96117011.5、 02110649.5):利用热胀冷缩的原理,花粉经低温冷冻后迅速投入热水中"炸裂",这种方法对花粉的营养成分破坏较大,且操作复杂。 Currently Pollen method domestic and international coverage are the following: (1) broken temperature difference method (Patent Application No. 96117011.5, 02110649.5): using the principle of thermal expansion and contraction, after freezing the pollen quickly into hot water "burst "this method of destruction of nutrients larger pollen, and complex operation. (2) 机械破壁法(专利申请号86103261、 90108303. 8、 95110207. 9、 96117168. 5) 是将花粉用水调成液体,再通过胶体磨、高压均质机等机械进行破壁。 (2) mechanical breakage method (Patent Application No. 86103261, 90108303.8, 95110207.9, 96117168.5) pollen is transferred into the liquid water, then broken through a colloid mill, high pressure homogenizer and other machinery. 使用这种方法破壁,花粉需经浸湿成液体后才能处理,操作复杂。 Using this method broken, pollen subject soaked into a liquid to process, complicated operations. (4)发酵酶解破壁法(专利申请号03115992.3、 87104508、 91106215.7、 95103910.5、 98104558.8、 02106399.0)是一种应用较广泛的方法,利用花粉自身丰富的微生物或通过接种微生物产生的酶类,使花粉内含物降解,渗透压升高而使花粉破壁,该方法破壁所需的时间长,且发酵过程中易被杂菌污染而影响质量。 (4) Fermentation broken enzymatic method (Patent Application No. 03115992.3, 87104508, 91106215.7, 95103910.5, 98104558.8, 02106399.0) is an application of the broader approach, using its own pollen rich microorganisms or enzymes produced by microbial inoculation, so pollen degradation inclusions, the osmotic pressure pollen, long time required for the process broken, and the bacterial contamination during fermentation easily affect the quality. 以上破壁方法均为湿法破壁,要求用不同的溶剂将花粉润湿或调成液体,破壁后若制成固体制剂必须进行干燥,造成产品成本的增加。 The method of wet broken broken above are required with different solvents or wetting pollen into a liquid, when a solid preparation must be broken after drying, resulting in increased product cost. (5) 微波辐射破壁法(专利申请号200710022400.2)是将袋装花粉置于微波炉内,加热烘烤。 (5) Method broken microwave radiation (Patent Application No. 200710022400.2) is placed in a microwave bag pollen, heating and baking. 该方法使花粉粒整体不遭破坏,但袋中心与表层的温度不易控制,工艺复杂,生产效率低。 This method enables the whole pollen grains is not destroyed, but the temperature of the surface layer and the center of the pouch is difficult to control, complex process, low production efficiency. (6) 气流粉碎法(专利申请号01115014. 9)是利用压縮空气泵空气产生高压气流,经喷嘴经音速喷入粉碎室,通过碰撞,在低温下达到粉碎花粉的目的。 (6) gas stream pulverizing method (Patent Application No. 01115014.9) generating a high pressure gas stream is an air pump compressed air through the nozzle by the velocity of sound is injected into the grinding chamber, through collisions, pollen purpose pulverized at a low temperature. 该方法操作较复杂,破壁后的花粉内含物完全裸露于外界环境中,容易产生氧化变质。 The method is more complicated, the pollen contents broken completely exposed to the outside environment, prone to oxidative deterioration. 传统的破壁方法各有其优点,但是缺点同样明显,或者处理周期长,如冷热交替处理法和自溶法等,在生产中使用不便;或者破壁过程中产生大量热量, 导致花粉酶活的丧失,如各种机械方法破壁;或者效率高但成本昂贵,如酶法消化法、高压均质处理和高压电场方法,大大增加产品成本,在生产中无法推广使用。 Broken conventional methods have their advantages, but the disadvantage is also obvious, or long processing cycle, alternating hot and cold treatment method as autolysis and the like, used in the production of the inconvenience; or broken during a lot of heat, resulting in pollen enzyme live loss of mechanical methods such as various broken; or efficient but costly, such as enzymatic digestion, high pressure homogenization and high electric field processing methods greatly increases the cost of the product, can not promote the use in production. 发明内容本发明的目的是为了克服己有技术的缺点,提供一种处理成本低,操作简便,能使花粉粒整体不遭破坏,细胞破壁速度快且破壁率高,能够在生产中应用的蜂花粉超临界二氧化碳破壁方法。 Object of the present invention is to overcome the drawbacks of the prior art has provided a low processing cost, simple operation, whole pollen grains can not be destroyed, broken fast cell wall and high speed, can be used in production bee pollen broken supercritical carbon dioxide method. 本发明的蜂花粉超临界二氧化碳破壁方法,其特征在于:将蜂花粉的水分含量控制在4〜20%,放入超临界二氧化碳萃取装置的萃取釜中,控制二氧化碳温度32〜50。 Bee pollen broken supercritical carbon dioxide method of the present invention is characterized in that: the moisture content is controlled to bee pollen 4~20%, and extracted into supercritical carbon dioxide extraction vessel means, the control temperature of 32~50 carbon dioxide. C,压力8〜50MPa,作用5〜30分钟,打开排气阀迅速排空二氧化碳,收集破壁花粉即可。 C, pressure 8~50MPa, the role of 5~30 minutes, opening the exhaust valve is rapidly vented carbon dioxide, can be broken pollen collected. 超临界C02萃取装置详见图1: 1.C02钢瓶;2.净化器;3.储罐(冷箱);4混合器;5.净化器;6萃取釜;7.排气阀;8.分离釜;9.压力表;IO.流量计本发明的优点:1、 本发明为干法破壁,破壁花粉无需干燥处理,去除了干燥工序对花粉有效成分影响的可能。 C02 supercritical extraction apparatus See Figure 1: 1.C02 cylinder; 2 scrubber; 3 tank (cold box); mixer 4; 5 purifier; extraction vessel 6; 7 an exhaust valve; 8..... separation vessel; 9 gauge; flowmeter advantages of the present invention IO: 1, the present invention is a dry process broken, broken pollen without drying, to a drying step may affect the active ingredients in addition to the pollen. 2、 本发明以超临界二氧化碳作为介质进行花粉细胞破壁,超临界二氧化碳易于渗透到细胞内,很快就达到细胞内外的压力平衡;然后突然降压,此时细胞因胞内外压差较大,剧烈膨胀而发生破裂,达到既破壁又灭菌的效果。 2, the present invention is carried out in supercritical carbon dioxide as the cell wall of pollen medium, supercritical carbon dioxide easily penetrates into cells, soon reached equilibrium pressure inside and outside the cell; then suddenly down, some large intracellular cytokine external pressure , severe swelling and rupture, to achieve both broken and sterilization effect. 3、 本发明中花粉整体没有被破坏,内含物在干燥条件下仍存在于破裂的花粉壁内,有利于营养成分保存。 3, the present invention is not destroyed whole pollen, the contents still present within the rupture of pollen wall, beneficial nutrients stored under dry conditions. 4、 本发明为低温、短时破壁,整个过程在较低温度(5(TC以下)下进行,破壁时间短(30分钟以内),减少了产品的受热变性影响,使活性成分保存完全。5、 本发明工作压力较低(50MPa以下),流程简单,大大降低了设备的投资,提高了生产安全性;二氧化碳是一种不活泼的气体,破壁过程中不发生化学反应, 且属于不燃性气体,无味、无臭、无毒,安全性好,对环境无污染。6、 本发明操作简便,生产效率高,节约能源,不产生污染环境的废物,设备运行费用低,能耗少,生产成本低,非常适合于工业化大批量生产,是一种理想的花粉破壁方法。电镜观察详见附图说明-图2未破壁花粉电镜形态图3经本发明方法破壁后花粉细胞破壁率高达95%以上图4经本方法破壁后花粉细胞壁不同程度破裂,内容物存在于破碎的花粉壁中具体实施方式,以下结合实施 4, the present invention is a low temperature, short broken, the entire process is performed at a relatively low temperature (5 (TC or lower), broken short time (30 minutes), to reduce the influence of heat denaturation of the product, stored in a fully active ingredient .5, it is low (less 50 MPa) operating pressure of the present invention, the process is simple, greatly reducing the equipment investment, increase production safety; carbon dioxide is an inert gas, a chemical reaction occurs during broken, and belonging to nonflammable gas, tasteless, odorless, non-toxic, safety, environmental pollution .6, the present invention is easy to operate, high production efficiency, energy conservation, waste does not pollute the environment, low equipment operating costs, low energy consumption low production cost, very suitable for industrial mass production, is an ideal method of electron microscopy pollen BRIEF DESCRIPTION see - FIG. 2 pOLLEN morphology FIG 3 is not broken by the method of the present invention is broken pollen cells broken rate of 95% Figure 4 after rupture of cell walls of varying degrees of the method of pollen broken, crushed present in the content of pollen wall DETAILED DESCRIPTION embodiment, in conjunction with the following embodiments 例进一步说明本发明。实施例1:将新鲜蜂花粉真空干燥至水分含量为6. 20%,取300g干燥花粉装入1L萃取器,在萃取釜温度35"C的条件下,用纯度为99%的二氧化碳进行升压至萃取釜压力15MPa;保持压力5min后打开萃取罐排气阀迅速排空二氧化碳,收集花粉即可。经电镜检测,花粉细胞已破壁。实施例2:称取干燥蜂花粉300g装入lL萃取器,在萃取釜温度35"C的条件下,用纯度为99%的二氧化碳进行升压至萃取釜压力30MPa;保持压力5min后打开萃取罐排气阀迅速排空二氧化碳,收集花粉即可。经电镜检测,花粉细胞已破壁。 实施例3:将新鲜蜂花粉真空干燥至水分含量为6. 20%,取干燥后花粉300g装入1L萃取器,在萃取釜温度4(TC的条件下,用纯度为99%的二氧化碳进行升压至萃取釜压力30MPa;保持压力10min后打开萃取罐排气阀迅速排空二氧化碳;取出花粉即可。经电镜检测,花粉细胞 Examples further illustrate the present invention Example 1: The fresh pollen vacuum dried to a moisture content of 6.20%, taking pollen charged 300g dried 1L extractor, the extraction kettle temperature at 35 "condition C, with a purity of 99 % of carbon dioxide the extraction pressure was raised to 15MPa; holding pressure extraction tank vent valve is opened is rapidly vented carbon dioxide, can be collected by the electron microscope pollen, pollen cells have been broken after 5min Example 2: Weigh dried bee. lL extractor charged with 300g of pollen, under "conditions of the extraction vessel temperature of 35 C, 99% of boosting the purity of carbon dioxide to the extraction pressure was 30MPa; holding pressure after 5min open extraction tank vent valve is rapidly vented carbon dioxide, collected by electron microscopy to pollen, pollen cells have been broken Example 3: the fresh pollen dried in vacuo to a moisture content of 6.20%, the charged 300g of dried pollen 1L extractor, the extraction temperature in the autoclave 4 under (conditions of TC, 99% carbon dioxide pressure was raised to 30MPa extracted with purity; open holding pressure after 10min extraction tank vent valve is rapidly vented carbon dioxide; can be taken by the electron microscope pollen, pollen cells. 破壁。 实施例4:干燥蜂花粉300g装入1L萃取器,在萃取釜温度4(TC的条件下,用纯度为99%的二氧化碳进行升压至萃取釜压力45MPa;保持压力10min后打开萃取罐取出花粉即可。经电镜检测,花粉细胞已破壁。 实施例5:将花粉粒真空干燥至水分含量为6. 20%,将干燥后的花粉300g装入1L萃取器,在萃取釜温度45"C的条件下,用纯度为99%的二氧化碳进行升压至萃取釜压力5MPa;保持压力30min后打开萃取罐排气阀迅速排空二氧化碳,取出花粉。 经电镜检测,花粉细胞已破壁。 Broken Example 4: 300g charged pollen dried 1L extractor, the extraction vessel at a temperature of 4 (the TC conditions, with a purity of 99% carbon dioxide extraction pressure was raised to 45MPa; open holding pressure after 10min and extracted the tank can be removed by electron microscopy pollen, pollen cells have been broken Example 5: the pollen grains vacuum dried to a moisture content of 6.20%, the pollen was charged 300g of dried 1L extractor, the extraction temperature in the autoclave 45 "under the condition C, carried out with a purity of 99% carbon dioxide extraction pressure was raised to 5 MPa; holding pressure extraction tank vent valve is opened is rapidly vented carbon dioxide, remove pollen 30min by electron microscopy, pollen cells has been broken. .

Claims (5)

1. 蜂花粉超临界二氧化碳破壁方法,其特征在于:将蜂花粉的水分含量控制在4~20%,装入超临界二氧化碳萃取装置的萃取釜中,通入二氧化碳加压进行花粉细胞破壁,其超临界二氧化碳流体花粉细胞破壁技术的各参数范围分别为:细胞破壁压力为8~50MPa,破壁温度32~50℃,时间5~30分钟;然后打开排气阀迅速排空二氧化碳,从而使花粉细胞外壁因壁内外压力差较大而发生破裂。 1. Bee Pollen broken supercritical carbon dioxide, characterized in that: the moisture content is controlled to bee pollen from 4 to 20%, the extraction kettle was charged supercritical carbon dioxide extraction apparatus, the pressurized carbon dioxide into pollen cell wall each parameter range of supercritical fluid pollen cells were broken technology: cell wall pressure of 8 ~ 50MPa, broken temperature 32 ~ 50 ℃, for 5 to 30 minutes; and then opening the exhaust valve is rapidly vented carbon dioxide , so that the outer wall of pollen cells due to the large difference in pressure inside and outside wall rupture.
2. 根据权利要求1所述的蜂花粉破壁方法,其特征在于:所述蜂花粉为商用或非商用蜂花粉的任意品种,不受花粉种类的限制。 Bee Pollen The method according to claim 1, wherein: said bee pollen or any commercial varieties of commercial bee pollen, pollen species without limitation.
3. 根据权利要求1所述的蜂花粉破壁方法,其特征在于:细胞破壁压力为8〜50MPa,优选30〜40MPa。 3. Bee Pollen method of claim 1, wherein: a pressure cell wall 8~50MPa, preferably 30~40MPa.
4. 根据权利要求1所述的蜂花粉破壁方法,其特征在于:破壁所需温度为30〜50。 Bee Pollen 4. The method according to claim 1, wherein: the desired temperature of 30 ~ 50 broken. C,优选35〜40。 C, preferably 35~40. C。 C.
5. 根据权利要求1所述的蜂花粉破壁方法,其特征在于:破壁所需压力保持时间为5〜30分钟,优选15〜25分钟。 Bee Pollen 5. The method according to claim 1, wherein: the pressure holding time required broken 5~30 minutes, preferably 15~25 minutes.
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