WO2017080520A1 - Method for extracting avermectin b2 from avermectin ointment - Google Patents
Method for extracting avermectin b2 from avermectin ointment Download PDFInfo
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- WO2017080520A1 WO2017080520A1 PCT/CN2016/105554 CN2016105554W WO2017080520A1 WO 2017080520 A1 WO2017080520 A1 WO 2017080520A1 CN 2016105554 W CN2016105554 W CN 2016105554W WO 2017080520 A1 WO2017080520 A1 WO 2017080520A1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/08—Hetero rings containing eight or more ring members, e.g. erythromycins
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- the invention relates to the technical field of antibiotic extraction, in particular to a method for extracting and preparing avermectin.
- Abamectin is a low-toxic, high-efficiency and highly selective environmentally friendly insecticide, making it an ideal pesticide product to replace traditional high-toxic pesticides.
- Avermectin is a group of similar 16-membered macrolide antibiotics isolated from the fermentation products of Streptomyces griseus. This group contains 8 homologous components with similar structures, of which B 1 ( The components containing B 1 a, B 1 b) and B 2 (containing B 2 a, B 2 b) are the most abundant and most active components.
- the main product currently on the market is avermectin B 1 . .
- the existing extraction process of avermectin is obtained by filtering, concentrating and crystallization of the fermentation broth to obtain crude avermectin.
- the filtrate obtained by suction filtration is a crude mother liquor, and the crude mother liquor is concentrated and desolved to obtain avermectin ointment. .
- avermectin raw powder - avermectin ointment contains about 5% avermectin B 1 a, 30% avermectin B 2 and toluene as a diluent, and some Polysaccharides and solid lipid impurities are complex and highly toxic compared to the original powder, so they cannot be treated as waste.
- the B 2 component contained in the avermectin ointment is more effective than the B 1 component, wherein the B 2 a component has the strongest activity, and the control effect on the pests such as nematodes and lepidoptera is better.
- the existing process for extracting the B 2 component from the ointment is: adding toluene to the ointment, filtering down the crude B 2 by cooling, and obtaining the B 2 fine by five repeated crystallizations.
- Five times of recrystallization has a large loss of solvent, generally 7kg of toluene per kilogram of avermectin B 2 product. Because of the safety hazard of toluene volatilization into the air, it is easy to cause environmental pollution and cannot be recycled and reused.
- the process also has problems such as insufficient purity of the product (the highest B 2 content can only reach 91%) and complicated process steps.
- the technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a method for extracting avermectin B 2 from avermectin ointment, which uses activated carbon and common organic solvent to extract avermectin ointment.
- the B 2 component has the characteristics of simple process, energy saving and environmental protection.
- a method for extracting avermectin B2 from avermectin ointment comprises the following steps:
- the avermectin ointment is dissolved in a crystallization solvent, the temperature is lowered to -6 ° C to -10 ° C to precipitate crystals, vacuum filtration to obtain crude avermectin B 2;
- avermectin B2 fine The crude avermectin B2 obtained in the step a is dissolved in a crystallization solvent, deactivated by adding activated carbon, cooled to -6 ° C to -10 ° C, recrystallized, suction filtered, and dried to obtain avermectin B 2 fine.
- a method for extracting avermectin B2 from the above avermectin ointment wherein the volume ratio of the mass of the avermectin ointment to the crystallization solvent in the step a is 1:1 to 1:1.5; Acetone or methyl ethyl ketone.
- the method for extracting avermectin B2 from the above avermectin ointment wherein the volume ratio of the crude avermectin B2 to the crystallization solvent in the step b is 1:3-1:5; the quality of the activated carbon is 5% of the crude quality of avermectin B2.
- the invention uses the cheap activated carbon and the commonly used organic solvent to separate and purify the avermectin B 2 component from the avermectin ointment, the process is simple, the operation is convenient, the crystallization is reduced by three times compared with the prior art, and the purity is up to 99. % of avermectin B 2 product, wherein B 2 a is above 96%.
- the solvent acetone or methyl ethyl ketone has the characteristics of low boiling point and good viscosity reducing performance, and the heat required in the production process is small, thereby greatly reducing the energy consumption of steam, electricity and water, and saving operating costs.
- the above-mentioned process is used as a waste ointment in a comprehensive manner, and does not add harmful additional reagents such as toluene, and the solvent consumption is small, and has the advantages of economical application, energy saving and environmental protection.
- Step a The crude mother liquor of the crude avermectin is concentrated and desolventized to obtain a avermectin ointment having a moisture content of ⁇ 2.0% and containing no methanol.
- a crystallization solvent is added to the avermectin ointment, and the volume ratio of the mass of the ointment to the crystallization solvent is 1:1 to 1:1.5 (M/V); the crystallization solvent is acetone or butanone.
- Step b adding the crude avermectin B 2 obtained in the step a to the recrystallization dissolution tank, and adding the crystallization solvent to dissolve, the volume ratio of the crude product to the crystallization solvent is 1:3-1:5 (M/V). .
- the mass of the activated carbon used was 5% of the crude product.
- the avermectin B 2 solution was heated to 70-80 ° C for 30 min, decolorized and filtered. The filtrate after filtration was naturally cooled to 25 ° C, and forced to cool to -6 to -10 ° C for 2 hours with cold brine.
- the secondary crystallization of avermectin B 2 is obtained by vacuum filtration in a suction filter, and the filtrate (secondary mother liquor) is used as a crystallization solvent for the step a.
- the obtained secondary crystal product is subjected to the above dissolution, filtration, and crystallization steps, and the obtained three crystal products are dried by a boiling dryer, and the avermectin B 2 fine powder is ⁇ 1.0%.
- the crude avermectin B2 was dissolved in 450 mL of acetone, and 7.5 g of activated carbon was added to the temperature to 70 ° C for 30 min for decolorization and filtration.
- the filtrate was naturally cooled to 25 ° C in a crystallization tank, and cooled to -6 ° C with cold brine.
- the crystals were cultured in an hour, and vacuum filtered to obtain a secondary crystalline product of 90 g.
- the secondary crystalline product was subjected to three times of crystallization by adding 450 mL of acetone and 4.5 g of activated carbon to obtain a crystal product three times. After drying, 60 g of avermectin B 2 fine powder was obtained, wherein the B 2 content was 99.6%, and the B 2 a content was 97.2%.
- the crude avermectin B2 was further dissolved in 438 mL of methyl ethyl ketone, and 7.3 g of activated carbon was added for secondary crystallization to obtain 93 g of a secondary crystalline product. Further, 465 mL of acetone and 4.65 g of activated carbon were added for three times of crystallization. After the three crystal products were dried, 55 g of avermectin B 2 fine powder was obtained, wherein the B 2 content was 98.9%, and the B 2a content was 96.5%.
- the avermectin B 2 fine powder was detected by high performance liquid chromatography.
- Detecting step Weigh 0.03g powder and B 2 100ML volumetric flask, dissolved in methanol, constant volume. The solution was aspirated and injected into a high performance liquid chromatograph at a flow rate of 1.0 ml/min.
- the column temperature was 25 ° C at room temperature, and the injection volume was 20 vl.
- the detection was carried out according to the above chromatographic conditions, and the detection time was 30 min. Calculate the B 2 content according to the external standard method.
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Abstract
A method for extracting avermectin B2 from an avermectin ointment comprises: dissolving an avermectin ointment into a crystallizing solvent, separating crystals out by cooling, and performing vacuum filtrating, thus obtaining an avermectin B2 crude product; and dissolving the avermectin B2 crude product into the crystallizing solvent, adding activated carbon for decoloration, and filtrating and drying after recrystallizing, thus obtaining an avermectin B2 fine product. The technology adopts cheap activated carbon and a common organic solvent for separating and purifying an avermectin B2 component from avermectin ointment, the technology is simple, the operation is convenient, crystallizing frequency is reduced, and a high-purity avermectin B2 product can be obtained.
Description
本发明涉及抗生素提取技术领域,特别是一种阿维菌素的提取制备方法。The invention relates to the technical field of antibiotic extraction, in particular to a method for extracting and preparing avermectin.
阿维菌素是一种低毒、高效、高选择性的环保型杀虫剂,使其成为代替传统高毒农药的理想农药产品。阿维菌素是由灰色链霉菌的发酵产物分离提取得到的一组结构类似的十六元大环内酯类抗生素,这一组中含有结构相近的8个同系物组分,其中B1(含有B1a、B1b)和B2(含有B2a、B2b)组分是含量最多、药物活性最强的组分,目前市场上主要开发的产品为阿维菌素B1。现有阿维菌素的提取工艺为发酵液经过滤、浓缩、结晶抽滤后得阿维菌素粗品,抽滤所得滤液为粗品母液,粗品母液经浓缩脱溶剂后得阿维菌素油膏。Abamectin is a low-toxic, high-efficiency and highly selective environmentally friendly insecticide, making it an ideal pesticide product to replace traditional high-toxic pesticides. Avermectin is a group of similar 16-membered macrolide antibiotics isolated from the fermentation products of Streptomyces griseus. This group contains 8 homologous components with similar structures, of which B 1 ( The components containing B 1 a, B 1 b) and B 2 (containing B 2 a, B 2 b) are the most abundant and most active components. The main product currently on the market is avermectin B 1 . . The existing extraction process of avermectin is obtained by filtering, concentrating and crystallization of the fermentation broth to obtain crude avermectin. The filtrate obtained by suction filtration is a crude mother liquor, and the crude mother liquor is concentrated and desolved to obtain avermectin ointment. .
作为阿维菌素原粉的副产物—阿维菌素油膏中约含有5%的阿维菌素B1a、30%的阿维菌素B2和作为稀释剂的甲苯,还有一些多糖和固态脂类杂质,成份较为复杂且毒性较原粉高,因此不能作为废物进行一般处理。阿维菌素油膏中含有的B2组分其药效高于B1组分,其中以B2a组分活性最强,对线虫、鳞翅目等害虫的防治效果更优。现有的从油膏中提取B2组分的工艺为:油膏中加入甲苯,降温抽滤出B2粗品,通过五次重复结晶得到B2精品。五次重结晶对于溶媒的损耗量大,一般为每公斤阿维菌素B2产品消耗7kg甲苯,由于甲苯挥发到空气中存在安全隐患,易造成环境污染,而且无法回收再利用,同时这种工艺还存在产品纯度不够高(B2含量最高只能达到91%)及工艺步骤繁琐等问题。As a by-product of avermectin raw powder - avermectin ointment contains about 5% avermectin B 1 a, 30% avermectin B 2 and toluene as a diluent, and some Polysaccharides and solid lipid impurities are complex and highly toxic compared to the original powder, so they cannot be treated as waste. The B 2 component contained in the avermectin ointment is more effective than the B 1 component, wherein the B 2 a component has the strongest activity, and the control effect on the pests such as nematodes and lepidoptera is better. The existing process for extracting the B 2 component from the ointment is: adding toluene to the ointment, filtering down the crude B 2 by cooling, and obtaining the B 2 fine by five repeated crystallizations. Five times of recrystallization has a large loss of solvent, generally 7kg of toluene per kilogram of avermectin B 2 product. Because of the safety hazard of toluene volatilization into the air, it is easy to cause environmental pollution and cannot be recycled and reused. The process also has problems such as insufficient purity of the product (the highest B 2 content can only reach 91%) and complicated process steps.
发明内容Summary of the invention
本发明所要解决的技术问题是克服已有技术之缺陷,提供一种阿维菌素油膏中提取阿维菌素B2的方法,它使用活性炭及常用有机溶剂提取阿维菌素油膏中的B2组分,具有工艺简单、节能环保的特点。
The technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a method for extracting avermectin B 2 from avermectin ointment, which uses activated carbon and common organic solvent to extract avermectin ointment. The B 2 component has the characteristics of simple process, energy saving and environmental protection.
本发明所述技术问题是以下述技术方案实现的:The technical problem of the present invention is achieved by the following technical solutions:
一种阿维菌素油膏中提取阿维菌素B2的方法,包括如下步骤:A method for extracting avermectin B2 from avermectin ointment comprises the following steps:
a、将阿维菌素油膏溶解于结晶溶剂中,降温至-6℃至-10℃析出结晶,真空抽滤得到阿维菌素B2粗品;a, the avermectin ointment is dissolved in a crystallization solvent, the temperature is lowered to -6 ° C to -10 ° C to precipitate crystals, vacuum filtration to obtain crude avermectin B 2;
b、将步骤a获得的阿维菌素B2粗品溶解于结晶溶剂中,加入活性炭进行脱色,降温至-6℃至-10℃重结晶后抽滤、干燥,得到阿维菌素B2精品。b. The crude avermectin B2 obtained in the step a is dissolved in a crystallization solvent, deactivated by adding activated carbon, cooled to -6 ° C to -10 ° C, recrystallized, suction filtered, and dried to obtain avermectin B 2 fine.
上述阿维菌素油膏中提取阿维菌素B2的方法,所述步骤a中阿维菌素油膏的质量与结晶溶剂的体积比为1:1-1:1.5;所述结晶溶剂为丙酮或丁酮。a method for extracting avermectin B2 from the above avermectin ointment, wherein the volume ratio of the mass of the avermectin ointment to the crystallization solvent in the step a is 1:1 to 1:1.5; Acetone or methyl ethyl ketone.
上述阿维菌素油膏中提取阿维菌素B2的方法,所述步骤b中阿维菌素B2粗品的质量与结晶溶剂的体积比为1:3-1:5;加入活性炭的质量为阿维菌素B2粗品质量的5%。The method for extracting avermectin B2 from the above avermectin ointment, wherein the volume ratio of the crude avermectin B2 to the crystallization solvent in the step b is 1:3-1:5; the quality of the activated carbon is 5% of the crude quality of avermectin B2.
上述阿维菌素油膏中提取阿维菌素B2的方法,重复进行步骤b中溶解、过滤和重结晶的步骤,经干燥得到阿维菌素B2精品。。The method for extracting avermectin B2 from the above avermectin ointment, repeating the steps of dissolving, filtering and recrystallizing in step b, and drying to obtain avermectin B2. .
本发明采用廉价的活性炭及常用的有机溶剂从阿维菌素油膏中分离提纯阿维菌素B2组分,工艺简单、操作方便,较现有工艺减少三次结晶,并可获得纯度高达99%的阿维菌素B2产品,其中B2a达到96%以上。所用溶剂丙酮或丁酮具有沸点低,降粘性能好的特点,生产过程中需要的热量小,因此大大降低了蒸汽、电、水的能耗,节约运营成本。上述工艺在综合回收利用作为废弃物油膏的同时,不添加甲苯等有害的附加试剂,溶媒消耗少,具有经济适用、节能环保的优点。The invention uses the cheap activated carbon and the commonly used organic solvent to separate and purify the avermectin B 2 component from the avermectin ointment, the process is simple, the operation is convenient, the crystallization is reduced by three times compared with the prior art, and the purity is up to 99. % of avermectin B 2 product, wherein B 2 a is above 96%. The solvent acetone or methyl ethyl ketone has the characteristics of low boiling point and good viscosity reducing performance, and the heat required in the production process is small, thereby greatly reducing the energy consumption of steam, electricity and water, and saving operating costs. The above-mentioned process is used as a waste ointment in a comprehensive manner, and does not add harmful additional reagents such as toluene, and the solvent consumption is small, and has the advantages of economical application, energy saving and environmental protection.
下面结合实施例对本发明作进一步详细说明。The present invention will be further described in detail below with reference to the embodiments.
步骤a、将提出阿维菌素粗品的粗品母液浓缩、脱溶剂,得到水分含量≤2.0%并且不含甲醇的膏状物即为阿维菌素油膏。阿维菌素油膏中加入结晶溶剂,油膏的质量与结晶溶剂的体积比为1:1-1:1.5(M/V);所述结晶溶剂为丙酮或丁酮。升温至70-80℃搅拌2小时,充分溶解为无粘度的均一液体,自然降温至25℃,使用冷盐水继续降温至-6至-10℃保温2小时养晶,保持低温状态在抽滤器中真空抽滤得到阿维菌素B2粗品,滤液(即一次母液)经浓缩脱溶剂后处理。
Step a: The crude mother liquor of the crude avermectin is concentrated and desolventized to obtain a avermectin ointment having a moisture content of ≤2.0% and containing no methanol. A crystallization solvent is added to the avermectin ointment, and the volume ratio of the mass of the ointment to the crystallization solvent is 1:1 to 1:1.5 (M/V); the crystallization solvent is acetone or butanone. Warm up to 70-80 ° C for 2 hours, fully dissolve into a non-viscosity uniform liquid, naturally cool to 25 ° C, use cold brine to continue to cool down to -6 to -10 ° C for 2 hours to keep the crystal, keep the low temperature in the suction filter The crude avermectin B 2 is obtained by vacuum filtration, and the filtrate (ie, one mother liquid) is subjected to concentration and solvent removal.
步骤b、将步骤a获得的阿维菌素B2粗品加入到重结晶溶解罐内,加入结晶溶剂溶解,粗品的质量与结晶溶剂的体积比为1:3-1:5(M/V)。后加入活性炭,所用活性炭的质量为粗品质量的5%。将阿维菌素B2溶解液升温至70-80℃保温30min,进行脱色、过滤,过滤后的滤液自然降温至25℃,使用冷盐水强制降温至-6至-10℃保温2小时养晶,在抽滤器中真空抽滤得到阿维菌素B2的二次结晶,滤液(二次母液)进入一次结晶套用即作为步骤a的结晶溶剂使用。将所得二次结晶产物重复上述溶解、过滤、结晶步骤,所得的三次结晶产物经沸腾干燥机烘干,干燥失重≤1.0%即为阿维菌素B2精粉。Step b, adding the crude avermectin B 2 obtained in the step a to the recrystallization dissolution tank, and adding the crystallization solvent to dissolve, the volume ratio of the crude product to the crystallization solvent is 1:3-1:5 (M/V). . After the addition of activated carbon, the mass of the activated carbon used was 5% of the crude product. The avermectin B 2 solution was heated to 70-80 ° C for 30 min, decolorized and filtered. The filtrate after filtration was naturally cooled to 25 ° C, and forced to cool to -6 to -10 ° C for 2 hours with cold brine. The secondary crystallization of avermectin B 2 is obtained by vacuum filtration in a suction filter, and the filtrate (secondary mother liquor) is used as a crystallization solvent for the step a. The obtained secondary crystal product is subjected to the above dissolution, filtration, and crystallization steps, and the obtained three crystal products are dried by a boiling dryer, and the avermectin B 2 fine powder is ≤1.0%.
实施例1Example 1
称阿维菌素油膏300g到结晶罐中,加入330mL结晶溶剂丙酮升温至75℃搅拌2小时,完全溶解后自然降温至25℃,使用冷盐水继续降温至-6℃保温2小时,保持低温状态放至抽滤器用真空抽滤得到阿维菌素B2粗品150g。Weigh 300g of avermectin ointment into the crystallization tank, add 330mL of crystallization solvent acetone and raise the temperature to 75 ° C and stir for 2 hours. After completely dissolving, naturally cool down to 25 ° C, continue cooling to -6 ° C for 2 hours with cold brine, keep the temperature low. The state was placed in a suction filter and vacuum filtered to obtain 150 g of crude avermectin B2.
将阿维菌素B2粗品加入450mL丙酮溶解,加入7.5g活性炭升温至70℃保温30min,进行脱色、过滤,滤液进入结晶罐中自然降温至25℃,使用冷盐水强制降温至-6℃保温2小时养晶,经真空抽滤得二次结晶产物90g。将二次结晶产物加450mL丙酮和4.5g活性炭进行三次结晶,得三次结晶产物。烘干后得到阿维菌素B2精粉60g,其中B2含量为99.6%,B2a含量97.2%。The crude avermectin B2 was dissolved in 450 mL of acetone, and 7.5 g of activated carbon was added to the temperature to 70 ° C for 30 min for decolorization and filtration. The filtrate was naturally cooled to 25 ° C in a crystallization tank, and cooled to -6 ° C with cold brine. The crystals were cultured in an hour, and vacuum filtered to obtain a secondary crystalline product of 90 g. The secondary crystalline product was subjected to three times of crystallization by adding 450 mL of acetone and 4.5 g of activated carbon to obtain a crystal product three times. After drying, 60 g of avermectin B 2 fine powder was obtained, wherein the B 2 content was 99.6%, and the B 2 a content was 97.2%.
实施例2Example 2
称阿维菌素油膏300g,加入400mL结晶溶剂丁酮升温至80℃搅拌2小时,完全溶解后降温至-10℃保温2小时,抽滤,得阿维菌素B2粗品146g。300 g of avermectin ointment was added, 400 mL of crystallizing solvent butanone was added to the mixture to raise the temperature to 80 ° C for 2 hours, completely dissolved, and then cooled to -10 ° C for 2 hours, and suction filtered to obtain 146 g of crude avermectin B2.
将阿维菌素B2粗品再加438mL丁酮溶解,加入7.3g活性炭进行二次结晶,得二次结晶产物93g。再加465mL丙酮和4.65g活性炭进行三次结晶,三次结晶产物烘干后得到阿维菌素B2精粉55g,其中B2含量为98.9%,B2a含量96.5%。The crude avermectin B2 was further dissolved in 438 mL of methyl ethyl ketone, and 7.3 g of activated carbon was added for secondary crystallization to obtain 93 g of a secondary crystalline product. Further, 465 mL of acetone and 4.65 g of activated carbon were added for three times of crystallization. After the three crystal products were dried, 55 g of avermectin B 2 fine powder was obtained, wherein the B 2 content was 98.9%, and the B 2a content was 96.5%.
阿维菌素B2精粉采用高效液相色谱仪进行检测,色谱检测条件为流动相(乙腈:甲醇:水=38:38:24),检测及其波长(UV=245nm),色谱柱为(VP-OD8 C18 250×4.6mm)。检测步骤为:称取B2精粉0.03g与100ML容量瓶中,用甲醇溶解,定容。吸取溶解液,注入高效液相色谱仪,流速1.0ml/min,柱温为室温25℃,进样量20vl,按以上色谱条件检测,检测时间30min。按外标法计算
B2含量。
The avermectin B 2 fine powder was detected by high performance liquid chromatography. The chromatographic conditions were mobile phase (acetonitrile:methanol:water=38:38:24), detection and wavelength (UV=245nm), and the column was (VP-OD8 C18 250×4.6mm). Detecting step: Weigh 0.03g powder and B 2 100ML volumetric flask, dissolved in methanol, constant volume. The solution was aspirated and injected into a high performance liquid chromatograph at a flow rate of 1.0 ml/min. The column temperature was 25 ° C at room temperature, and the injection volume was 20 vl. The detection was carried out according to the above chromatographic conditions, and the detection time was 30 min. Calculate the B 2 content according to the external standard method.
Claims (4)
- 一种阿维菌素油膏中提取阿维菌素B2的方法,其特征在于,包括如下步骤:A method for extracting avermectin B 2 from avermectin ointment, comprising the steps of:a、将阿维菌素油膏溶解于结晶溶剂中,降温至-6℃至-10℃析出结晶,真空抽滤得到阿维菌素B2粗品;a, the avermectin ointment is dissolved in a crystallization solvent, the temperature is lowered to -6 ° C to -10 ° C to precipitate crystals, vacuum filtration to obtain crude avermectin B 2 ;b、将步骤a获得的阿维菌素B2粗品溶解于结晶溶剂中,加入活性炭进行脱色,降温至-6℃至-10℃重结晶后抽滤、干燥,得到阿维菌素B2精品。b. The crude avermectin B 2 obtained in step a is dissolved in a crystallization solvent, deactivated by adding activated carbon, cooled to -6 ° C to -10 ° C, recrystallized, suction filtered, and dried to obtain avermectin B 2 .
- 根据权利要求1所述的阿维菌素油膏中提取阿维菌素B2的方法,其特征在于,所述步骤a中阿维菌素油膏的质量与结晶溶剂的体积比为1:1-1:1.5;所述结晶溶剂为丙酮或丁酮。The method for extracting avermectin B 2 from the avermectin ointment according to claim 1, wherein the volume ratio of the mass of the avermectin ointment to the crystallization solvent in the step a is 1: 1-1: 1.5; the crystallization solvent is acetone or methyl ethyl ketone.
- 根据权利要求2所述的阿维菌素油膏中提取阿维菌素B2的方法,其特征在于,所述步骤b中阿维菌素B2粗品的质量与结晶溶剂的体积比为1:3-1:5;加入活性炭的质量为阿维菌素B2粗品质量的5%。The method for extracting avermectin B 2 from the avermectin ointment according to claim 2, wherein the volume ratio of the crude avermectin B 2 to the crystallization solvent in the step b is 1 : 3-1:5; the mass of activated carbon added is 5% of the crude quality of avermectin B 2 .
- 根据权利要求3所述的阿维菌素油膏中提取阿维菌素B2的方法,其特征在于,重复进行步骤b中溶解、过滤和重结晶的步骤,经干燥得到阿维菌素B2精品。 The method for extracting avermectin B 2 from the avermectin ointment according to claim 3, wherein the step of dissolving, filtering and recrystallizing in step b is repeated, and avermectin B is obtained by drying. 2 boutique.
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CN106046085B (en) * | 2016-06-03 | 2018-12-04 | 河北兴柏农业科技有限公司 | A kind of processing method of abamectin ointment |
CN106977566A (en) * | 2017-04-20 | 2017-07-25 | 河北科技大学 | A kind of method that Avermectin B2 is extracted from abamectin ointment |
CN110105415A (en) * | 2019-04-15 | 2019-08-09 | 江苏物网慧农科技集团有限公司 | A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously |
CN111387179B (en) * | 2020-04-29 | 2021-11-12 | 河北威远生物化工有限公司 | Avermectin B2a solvation solid and preparation method thereof |
CN111606960A (en) * | 2020-05-15 | 2020-09-01 | 河北威远生物化工有限公司 | Avermectin B2a solvated crystal |
CN112574262A (en) * | 2020-11-29 | 2021-03-30 | 宁夏泰益欣生物科技有限公司 | Method for extracting and preparing abamectin B2 from abamectin primary crystallization mother liquor |
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