一种印楝素萃取方法 One kind of azadirachtin extraction method

技术领域 FIELD

[0001] 本发明涉及一种印楝素的萃取方法，特别涉及一种高纯度印楝素的萃取方法。 [0001] relates to an azadirachtin extraction process of the present invention, particularly relates to a method for the extraction of high purity azadirachtin.

背景技术 BACKGROUND

[0002] 近年来，我国农业高速发展，化学农药功不可没。 [0002] In recent years, the rapid development of China's agriculture, chemical pesticides contributed. 现有的化学农药对人畜健康有害，并不同程度地污染破坏环境和土壤。 Existing chemical pesticides harmful to human and animal health, and varying degrees of damage to the environment and soil pollution. 生物源性农药越来越为各国政府和农民所接受。 Biogenic pesticides more and more accepted by governments and farmers. 印楝素作为目前国际上公认的最有效和最安全的植物源性农作物及植物保护剂备受青睐。 Azadirachtin internationally recognized as the most effective and safest plant-derived crops and plant protection agents favored. 目前中国国内印楝素提纯工艺比较落后，纯度低于15 %。 At present, China's domestic azadirachtin purification process is relatively backward, less than 15% purity. 目前通常采用的乙醇法效率低；油性萃取法使得油性成分残留；高温法会对印楝素化学活性产生破坏性。 Ethanol is currently commonly used low efficiency; oily residues oily component extraction method makes; high temperature method would have a devastating chemical activity of azadirachtin. 因此，如何提高印楝素的纯度，从而提高印楝素的功效，成为该技术领域亟待解决的问题。 Therefore, how to improve the purity of azadirachtin, thereby increasing the effectiveness of azadirachtin, the technology sector problems to be solved. 发明内容 SUMMARY

[0003] 为了解决目前印楝素萃取纯度低，功效差的问题，本发明提出以下技术方案： [0003] In order to solve the azadirachtin extract of low purity, the problem of poor efficacy, the present invention proposes the following technical scheme:

[0004] 一种印楝素萃取方法，该方法主要包括以下步骤： [0004] A azadirachtin extraction method includes the following steps:

[0005] (I)将干燥的印楝果碾磨粉碎后溶于水中，搅拌均匀并沉淀； [0005] (I) The dry milling crushed neem fruit dissolved in water, stir and precipitation;

[0006] (2)将上述混合物进行分离得到提取液和沉淀物； [0006] (2) The above mixture was separated to obtain an extract and a precipitate;

[0007] (3)将沉淀物再次溶于水中搅拌均匀并沉淀，沉淀后进行分离，再次得到提取液和沉淀物； [0007] (3) The precipitate was again dissolved in water and stir the precipitate is separated after precipitation to obtain an extract and precipitate again;

[0008] (4)重复步骤（3)多次，收集多次得到的提取液； [0008] (4) repeating steps (3) repeatedly, many times resulting extract was collected;

[0009] (5)在提取液中加入疏水性的有机溶液并进行搅拌混合均匀； [0009] (5) was added to a solution of the hydrophobic organic extraction solution was stirred and mixed uniformly;

[0010] (6)待上述溶液中的有机溶剂与水层分开后，在该溶液中加入液态碳氢化合物，搅拌均匀并沉淀； [0010] (6) After the above-described organic solvent solution and the aqueous layer was separated from the liquid hydrocarbon was added to the solution, stir and precipitation;

[0011] (7)待上述溶液底部形成黄色的沉淀物，将该沉淀物分离出来并进行干燥，得到高纯度的印楝素。 [0011] (7) until the bottom of the solution a yellow precipitate formed, the precipitate was separated and dried to obtain high purity azadirachtin.

[0012] 作为本发明的一种优选方案，所述步骤（I)中水的重量为碾磨粉碎的印楝果重量的10〜30倍。 [0012] As a preferred embodiment of the present invention, said step (I) by weight of water is 10~30 times the milled pulverized neem fruit weight.

[0013] 作为本发明的另一种优选方案，所述步骤（5)中加入的有机溶液与提取液的重量比为I :15。 [0013] As a further preferred embodiment of the present invention, said step (5) was added to the solution and the weight of the organic extract ratio I: 15.

[0014] 作为本发明的再一种优选方案，所述步骤出）中的碳氢化合物重量为含有印楝素有机溶液的10〜15倍。 [0014] As still another preferred embodiment of the present invention, said step a) is 10 to 15 times the weight of the hydrocarbon-containing organic solution of azadirachtin.

[0015] 本发明带来的有益效果是：显著提高了印楝素的萃取浓度，得到纯度高的印楝素，生产成本低，易于操作，不破坏印楝素的药物活性；有效提高印楝素抗病虫害的效果。 [0015] The present invention brings beneficial effects: significantly increased the concentration of azadirachtin extraction, azadirachtin high purity, low production cost, easy to operate, does not destroy the pharmacological activity of azadirachtin; effectively improve the neem Su pest-resistant effect.

具体实施方式 DETAILED DESCRIPTION

[0016] 下面对本发明的较佳实施例进行详细阐述，以使本发明的优点和特征能更易于被本领域技术人员理解，从而对本发明的保护范围做出更为清楚明确的界定。 [0016] Next, the preferred embodiments of the present invention in detail, so that the advantages and features of the present invention can be more readily understood by those skilled in the art, and thus the scope of the present invention to make a more clear definition. [0017] 首先是印楝果干燥，粉碎碾磨干燥后的印楝果，分离出印楝果仁。 [0017] The first is the fruit dry neem, neem fruit after crushing mill drying isolated neem nuts. 得到的磨碎的印楝果仁中加入10〜30倍量的水，常温下20°C均匀搅拌大约10个小时。 Neem obtained milled nuts 10~30 times amount of water was added, at room temperature 20 ° C was stirred for about 10 hours uniformly. 然后静止3〜5个小时，直到沉淀完全。 Then still three to five hours, until complete precipitation. 之后通过滤过的方法分离出沉淀物。 Isolated by filtration after the precipitate. 印楝素有效成分溶解在水清液中。 Azadirachtin active ingredient is dissolved in clear water solution. 这时没有完全溶解的印楝果仁成分还会残留在沉淀物中，为提高印楝素的萃取量，分离出的沉淀物再用水重复萃取3〜4次。 At this time not completely dissolved neem kernels components may remain in the precipitate, to increase the extraction amount of azadirachtin, the separated precipitate is extracted repeatedly with water 3 to 4 times. 这样，印楝果仁中的大约85〜95%印楝素成分溶解在水清液中。 Thus, neem nuts about 85~95% azadirachtin ingredient is dissolved in clear water solution. 含有印楝素萃取物的水萃取将被进一步的提纯。 Aqueous extracts containing azadirachtin extract will be further purification.

[0018] 将疏水性的有机溶剂（如醋酸乙酯，己酸丁酯，丁酮，戊醇等）以I :15的倍量加入上一步骤获得的水萃取液中混合搅拌均匀，然后静止，直到加入的有机溶剂与水层分开，这个过程大约需要20个小时左右。 [0018] The hydrophobic organic solvent (e.g. ethyl acetate, butyl hexanoate, methyl ethyl ketone, amyl alcohol, etc.) to I: aqueous extract was added to 15 times the amount obtained in the previous step mixing evenly, then still The organic solvent is added until the aqueous layer separated, the process takes about 20 hours or so. 含有印楝素的有机溶液量大约是加入有机溶液量的1/4〜1/8。 The amount of organic solution containing azadirachtin organic solution was added an amount of about 1 / 4~1 / 8. 然后将10〜15倍量的液态碳氢化合物正已烷慢慢加入到含印楝素的浓缩有机溶液中并均匀搅拌，直到在容器底部形成黄白色的沉淀，与有机溶液慢慢分层，这时慢慢将无极性的有机溶液倒出。 Then 10 to 15 times the amount of liquid hydrocarbons n-hexane is slowly added to the organic solution containing azadirachtin is concentrated and uniformly stirred, until the bottom of the container yellow-white precipitate formed, and the organic solution was slowly layered, Then slowly pour nonpolar organic solution. 沉淀干燥后印楝素的含量可以达到40-60%。 After precipitation and drying azadirachtin content can reach 40-60%.

[0019] 以上所述，仅为本发明的具体实施方式,但本发明的保护范围并不局限于此，任何熟悉本领域的技术人员在本发明所揭露的技术范围内，可不经过创造性劳动想到的变化或替换，都应涵盖在本发明的保护范围之内。 [0019] The above are only specific embodiments of the present invention, but the scope of the present invention is not limited thereto, any skilled in the art within the technical scope of the invention disclosed, may inventive labor thought change or replace, should fall within the protection scope of the present invention. 因此，本发明的保护范围应该以权利要求书所限定的保护范围为准。 Accordingly, the scope of the invention should claim the scope of protection defined prevail.