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CN102702376A - Process for extracting chestnut polysaccharide by pressurized solvent extraction method - Google Patents

Process for extracting chestnut polysaccharide by pressurized solvent extraction method Download PDF

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Publication number
CN102702376A
CN102702376A CN2012101637910A CN201210163791A CN102702376A CN 102702376 A CN102702376 A CN 102702376A CN 2012101637910 A CN2012101637910 A CN 2012101637910A CN 201210163791 A CN201210163791 A CN 201210163791A CN 102702376 A CN102702376 A CN 102702376A
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extraction
chestnut
polysaccharide
extractor
diatomaceous earth
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王同坤
杨越冬
杜彬
梁雪
侯文龙
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Hebei Normal University of Science and Technology
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Hebei Normal University of Science and Technology
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Abstract

本发明公开了一种利用加压溶剂萃取方法提取板栗多糖的工艺。经将板栗仁烘干、粉碎与硅藻土充混合匀,装入萃取池中,再加入硅藻土填充,连接氮气、萃取仪和收集瓶装置,设置加压溶剂萃取仪条件:萃取温度50℃-70℃,加热时间4min-20min,萃取压强:3MPa-15MPa,循环次数:1-5次,淋洗体积40%-60%,氮吹时间40-100s萃取,将萃取液过滤,真空浓缩至1/4体积,去除蛋白,反复操作,直至分界面无白色混悬为止,加入75%-100%乙醇,醇沉5~12h,干燥得板栗多糖。本发明具有溶具剂用量少、操作简单快速、提高萃取效率,显著降低了单个样品的提取费用。同时保持了多糖物质的生物活性。The invention discloses a technique for extracting chestnut polysaccharide by using a pressurized solvent extraction method. After drying, crushing and mixing the chestnut kernels with diatomaceous earth, put them into the extraction tank, then add diatomaceous earth to fill, connect nitrogen, extraction instrument and collection bottle device, set the pressurized solvent extraction instrument conditions: extraction temperature 50 ℃-70℃, heating time 4min-20min, extraction pressure: 3MPa-15MPa, cycle times: 1-5 times, rinse volume 40%-60%, nitrogen blowing time 40-100s for extraction, filter the extract, and concentrate in vacuo To 1/4 volume, remove the protein, repeat the operation until there is no white suspension at the interface, add 75%-100% ethanol, alcohol precipitation for 5~12h, and dry to obtain chestnut polysaccharide. The invention has the advantages of less solvent consumption, simple and fast operation, improved extraction efficiency, and significantly reduces the extraction cost of a single sample. At the same time, the biological activity of the polysaccharide substance is maintained.

Description

一种利用加压溶剂萃取方法提取板栗多糖的工艺A process for extracting chestnut polysaccharides by means of pressurized solvent extraction

技术领域 technical field

本发明属于天然产物提取技术,具体说是涉及一种利用加压溶剂萃取(APLE)方法提取板栗多糖的工艺。 The invention belongs to the natural product extraction technology, in particular to a process for extracting chestnut polysaccharides by means of a pressurized solvent extraction (APLE) method.

背景技术 Background technique

原材料板栗(Castanea mollissima Blume),为壳斗科栗属。板栗多种植于山坡地,在欧洲、亚洲和美洲广泛种植,是我国传统种植的名优干果,唐代医学名家孙思邈曾说:“栗,肾之果也,肾病宜食之;生食治腰、脚不遂。”多糖是糖天然存在的重要形式,是一类具有生物生理活性和特殊保健功能的多糖类物质。具有增强机体免疫功能、抗氧化、抗衰老、抗肿瘤、抗病毒、抗突变、抗辐射和促进骨髓造血功能等重要生物活性。 The raw material chestnut (Castanea mollissima Blume) belongs to the genus Fagaceae. Chestnuts are mostly planted on hillsides and are widely planted in Europe, Asia and America. They are famous and high-quality dried fruits traditionally planted in my country. Sun Simiao, a famous medical doctor in Tang Dynasty, once said: "Chestnut is also the fruit of the kidney. Kidney disease should be eaten; raw food can treat waist and feet." Failure.” Polysaccharide is an important form of sugar naturally occurring, and it is a class of polysaccharides with biological and physiological activities and special health functions. It has important biological activities such as enhancing the immune function of the body, anti-oxidation, anti-aging, anti-tumor, anti-virus, anti-mutation, anti-radiation and promoting bone marrow hematopoietic function.

加压溶剂萃取技术是由Richter等(1995)提出的一种全新的方法。已被美国国家环保局(EPA)推荐为一种标准的萃取方法。本发明采用加压溶剂萃取技术与传统提取方法相比较具有溶剂用量少、操作简单快速,萃取效率显著提高,并且降低单个产品的提取费用,同时保持了多糖物质的生物活性等突出优点。尽管加压溶剂萃取技术是近几年才发展的新技术,但由于其特点突出,已受到分析化学界的极大关注。该技术已在环境、药物、食品、农业和聚合物工业等领域得到广泛应用。但是,利用加压溶剂萃取技术对板栗中多糖物质进行提取的方法目前尚未见有关这方面的报道。 The pressurized solvent extraction technique is a brand-new method proposed by Richter et al. (1995). It has been recommended by the US Environmental Protection Agency (EPA) as a standard extraction method. Compared with the traditional extraction method, the pressurized solvent extraction technology adopted by the present invention has the advantages of less solvent consumption, simple and fast operation, significantly improved extraction efficiency, and reduced extraction cost of a single product, while maintaining the biological activity of polysaccharides and other outstanding advantages. Although pressurized solvent extraction technology is a new technology developed in recent years, it has attracted great attention in the field of analytical chemistry due to its outstanding characteristics. This technology has been widely used in the fields of environment, medicine, food, agriculture and polymer industry. However, the method for extracting polysaccharides from chestnuts using pressurized solvent extraction technology has not yet been reported in this regard.

发明内容 Contents of the invention

本发明的目的是提供一种利用加压溶剂萃取方法提取板栗多糖的工艺。具有溶剂用量少、操作简单快速、提高萃取效率,显著降低了单个产品的提取费用。同时,还具有保持多糖物质的生物活性突出的优点。 The purpose of the present invention is to provide a process for extracting chestnut polysaccharides using a pressurized solvent extraction method. It has the advantages of less solvent consumption, simple and fast operation, improved extraction efficiency, and significantly reduces the extraction cost of a single product. At the same time, it also has the outstanding advantage of maintaining the biological activity of polysaccharide substances.

   本发明的提取板栗多糖的工艺,包括: The process of extracting chestnut polysaccharide of the present invention comprises:

   1、将板栗剥壳,取板栗仁烘干,温度为25℃-50℃,然后用粉碎机研磨成板栗粉,装入密封袋后,放入干燥器中,备用; 1. Shell the chestnuts, take the chestnut kernels and dry them at a temperature of 25°C-50°C, then grind them into chestnut powder with a grinder, put them into a sealed bag, put them in a desiccator, and set aside;

   2、取上述板栗粉与硅藻土充分混合均匀,装入萃取池中,然后再加入1~20 Kg硅藻土填满萃取池,连接好氮气装置、萃取仪和收集瓶; 2. Take the above-mentioned chestnut powder and diatomaceous earth and mix well, put it into the extraction pool, then add 1~20 Kg of diatomite to fill the extraction pool, and connect the nitrogen device, extraction instrument and collection bottle;

   3、分别打开氮气和萃取仪开关,萃取仪自检,用清洗溶剂清洗萃取仪管道,设定预热温度开始预热; 3. Turn on the switch of nitrogen gas and extractor respectively, self-check the extractor, clean the pipeline of the extractor with cleaning solvent, set the preheating temperature and start preheating;

   4、设置加压溶剂萃取仪条件:萃取温度50 ℃-70 ℃,设置加热时间4 min-20 min,萃取压强:3 MPa-15 MPa,设置循环次数:1-5次,淋洗体积40 %-60 %,氮吹时间40-100 s,开始萃取; 4. Set the conditions of the pressurized solvent extractor: extraction temperature 50 ℃-70 ℃, set heating time 4 min-20 min, extraction pressure: 3 MPa-15 MPa, set cycle times: 1-5 times, rinse volume 40% -60%, nitrogen blowing time 40-100 s, start extraction;

   5、萃取完成后,萃取液进入收集瓶,将萃取液过滤,真空浓缩至1/4体积,去除蛋白,反复操作,直至分界面无白色混悬为止,加入75 %-100 %乙醇,醇沉5~12 h,干燥得板栗多糖。 5. After the extraction is completed, the extract enters the collection bottle, filters the extract, concentrates in vacuum to 1/4 volume, removes the protein, and repeats the operation until there is no white suspension at the interface, then adds 75%-100% ethanol, and alcohol precipitation 5~12 h, dry chestnut polysaccharide.

在本发明中,所述步骤(2)中的板栗粉与硅藻土按20 Kg  :10~30 Kg的比例混合。 In the present invention, the chestnut powder in the step (2) is mixed with diatomaceous earth in a ratio of 20 Kg: 10-30 Kg.

本发明所指的清洗溶剂、萃取溶剂均为纯水。 The cleaning solvent and extraction solvent referred to in the present invention are both pure water.

因此,本发明通过上述板栗处理技术及多糖类物质的提取技术整合,可以达到快速、高效的多糖提取过程。具有提取溶剂用量少,萃取全过程用时短,萃取过程为静态萃取,提取到的挥发物质纯净完全,同时减少多糖物质的生物活性被破坏的可能。 Therefore, the present invention can achieve a fast and efficient polysaccharide extraction process through the integration of the above-mentioned chestnut processing technology and polysaccharide extraction technology. It has the advantages of less extraction solvent consumption, short extraction time in the whole extraction process, static extraction, and pure and complete extracted volatile substances, while reducing the possibility of destroying the biological activity of polysaccharide substances.

本发明的显著优点: Significant advantage of the present invention:

本发明采用全自动加压溶剂萃取(Automated Pressurized Liquid Extraction, APLE)方法提取板栗多糖。加压溶剂萃取方法与传统的索氏提取、超声提取、微波萃取方法相比,具有溶剂用量少、操作简单快速、提高萃取效率、连续性好,显著降低了单个产品的提取费用,还具有健康环保、自动化程度高,同时保持了多糖物质的生物活性的突出优点。 The present invention adopts automatic pressurized solvent extraction (Automated Pressurized Liquid Extraction, APLE) method to extract chestnut polysaccharide. Compared with the traditional Soxhlet extraction, ultrasonic extraction, and microwave extraction, the pressurized solvent extraction method has the advantages of less solvent consumption, simple and fast operation, improved extraction efficiency, good continuity, and significantly reduces the extraction cost of a single product. It is healthy, environmentally friendly, and highly automated, while maintaining the outstanding advantages of the biological activity of polysaccharides.

具体实施方式 Detailed ways

实施例1 Example 1

   1、将板栗剥壳、取板栗仁烘干,温度为25℃-50℃,然后用粉碎机研磨成板栗粉,装入密封袋后,放入干燥器中,备用; 1. Shell the chestnuts, take the chestnut kernels and dry them at a temperature of 25°C-50°C, then grind them into chestnut powder with a grinder, put them into a sealed bag, put them in a desiccator, and set aside;

   2、取上述处理的干燥板栗粉20 Kg与硅藻土10 Kg充分混合均匀,装入萃取池中,然后再加入10 Kg硅藻土填满萃取池,连接好氮气装置、萃取仪和收集瓶; 2. Take 20 Kg of the above-mentioned dried chestnut powder and 10 Kg of diatomaceous earth, mix well, put it into the extraction pool, then add 10 Kg of diatomaceous earth to fill the extraction pool, and connect the nitrogen device, extraction instrument and collection bottle ;

   3、分别打开氮气和仪器开关,等待仪器自检,自检完成后用清洗溶剂清洗萃取仪管道,设定预热温度开始预热; 3. Turn on the nitrogen gas and the instrument switch respectively, wait for the instrument self-inspection, after the self-inspection is completed, clean the extractor pipeline with a cleaning solvent, set the preheating temperature and start preheating;

   4、步骤3完成后,设置加压溶剂萃取仪条件:萃取温度50 ℃,设置加热时间4 min,萃取压强:3 MPa,设置循环次数:1,淋洗体积60 %,氮吹时间60 s,开始萃取; 4. After step 3 is completed, set the conditions of the pressurized solvent extractor: extraction temperature 50 °C, set heating time 4 min, extraction pressure: 3 MPa, set cycle times: 1, rinse volume 60%, nitrogen blowing time 60 s, start extraction;

   5、萃取完成后,萃取液进入收集瓶,取出收集瓶,将萃取液过滤,真空浓缩至1/4体积,去除蛋白,反复操作,直至分界面无白色混悬为止,加入75 %-100 %乙醇,醇沉5~12 h,干燥得板栗多糖。 5. After the extraction is completed, the extract enters the collection bottle, take out the collection bottle, filter the extract, concentrate in vacuum to 1/4 volume, remove the protein, and repeat the operation until there is no white suspension at the interface, add 75%-100% ethanol, alcohol precipitation for 5-12 h, and drying to obtain chestnut polysaccharide.

实施例2 Example 2

   1、同样采用实施例1的步骤1处理备用; 1. Also adopt step 1 of embodiment 1 to process for standby;

   2、取上述处理的干燥板栗粉20 Kg与硅藻土20 Kg充分混合均匀,装入萃取池中,然后再加入5 Kg硅藻土填满萃取池,连接好氮气装置、萃取仪和收集瓶; 2. Take 20 Kg of the above-mentioned dried chestnut powder and 20 Kg of diatomaceous earth, mix them evenly, put them into the extraction pool, then add 5 Kg of diatomaceous earth to fill the extraction pool, and connect the nitrogen device, extraction instrument and collection bottle ;

   3、分别打开氮气和萃取仪开关,等待萃取仪自检,自检完成后用清洗溶剂清洗萃取仪管道,设定预热温度开始预热; 3. Turn on the switch of nitrogen gas and extractor respectively, wait for the self-test of the extractor, after the self-test is completed, clean the pipeline of the extractor with cleaning solvent, set the preheating temperature and start preheating;

   4、完成步骤3后,设置加压溶剂萃取仪条件:萃取温度60 ℃,设置加热时间8 min,萃取压强:6 MPa,设置循环次数:2,淋洗体积60 %,氮吹时间60 s,开始萃取; 4. After completing step 3, set the conditions of the pressurized solvent extractor: extraction temperature 60 °C, set heating time 8 min, extraction pressure: 6 MPa, set cycle times: 2, rinse volume 60%, nitrogen blowing time 60 s, start extraction;

   5、萃取完成后,萃取液进入收集瓶,取出收集瓶,将萃取液过滤,真空浓缩至1/4体积,去除蛋白,反复操作,直至分界面无白色混悬为止,加入75 %-100 %乙醇,醇沉5~12 h,干燥得板栗多糖。 5. After the extraction is completed, the extract enters the collection bottle, take out the collection bottle, filter the extract, concentrate in vacuum to 1/4 volume, remove the protein, and repeat the operation until there is no white suspension at the interface, add 75%-100% ethanol, alcohol precipitation for 5-12 h, and drying to obtain chestnut polysaccharide.

实施例3 Example 3

   1、同样采用实施例1的步骤1处理备用; 1. Also adopt step 1 of embodiment 1 to process for standby;

   2、取上述处理的干燥板栗粉30 Kg与硅藻土15 Kg充分混合均匀,装入萃取池中,然后再加入5 Kg硅藻土填满萃取池。连接好氮气装置和萃取仪,将萃取池和收集瓶放在萃取仪指定位置; 2. Take 30 Kg of the above-mentioned dried chestnut powder and 15 Kg of diatomaceous earth, mix them well, put them into the extraction pool, and then add 5 Kg of diatomaceous earth to fill up the extraction pool. Connect the nitrogen device and the extractor, and place the extraction pool and collection bottle at the designated position of the extractor;

   3、分别打开氮气和萃取仪开关,等待萃取仪自检,自检完成后用清洗溶剂清洗萃取仪管道,设定预热温度开始预热; 3. Turn on the switch of nitrogen gas and extractor respectively, wait for the self-test of the extractor, after the self-test is completed, clean the pipeline of the extractor with cleaning solvent, set the preheating temperature and start preheating;

   4、完成步骤3后,设置加压溶剂萃取仪条件:萃取温度70 ℃,设置加热时间12 min,萃取压强:9 MPa,设置循环次数:3,淋洗体积60 %,氮吹时间60 s,开始萃取; 4. After completing step 3, set the conditions of the pressurized solvent extractor: extraction temperature 70 °C, set heating time 12 min, extraction pressure: 9 MPa, set cycle times: 3, rinse volume 60%, nitrogen blowing time 60 s, start extraction;

   5、萃取完成后,萃取液进入收集瓶,取出收集瓶,将萃取液过滤,真空浓缩至1/4体积,去除蛋白,反复操作,直至分界面无白色混悬为止,加入75 %-100 %乙醇,醇沉5~12 h,干燥得板栗多糖。 5. After the extraction is completed, the extract enters the collection bottle, take out the collection bottle, filter the extract, concentrate in vacuum to 1/4 volume, remove the protein, and repeat the operation until there is no white suspension at the interface, add 75%-100% ethanol, alcohol precipitation for 5-12 h, and drying to obtain chestnut polysaccharide.

实施例4 Example 4

   1、同样采用实施例1的步骤1处理备用; 1. Also adopt step 1 of embodiment 1 to process for standby;

   2、取上述处理的干燥板栗粉20 Kg与硅藻土30 Kg充分混合均匀,装入萃取池中,然后再加入5 Kg硅藻土填满萃取池,连接好氮气装置和萃取仪,将萃取池和收集瓶放在萃取仪指定位置; 2. Take 20 Kg of the above-mentioned dried chestnut powder and 30 Kg of diatomaceous earth, mix well, put it into the extraction pool, then add 5 Kg of diatomaceous earth to fill the extraction pool, connect the nitrogen device and the extraction instrument, and extract The pool and collection bottle are placed in the designated position of the extractor;

   3、分别打开氮气和萃取仪开关,等待萃取仪自检,自检完成后用清洗溶剂清洗萃取仪管道,设定预热温度开始预热; 3. Turn on the switch of nitrogen gas and extractor respectively, wait for the self-test of the extractor, after the self-test is completed, clean the pipeline of the extractor with cleaning solvent, set the preheating temperature and start preheating;

   4、完成步骤3后,设置加压溶剂萃取仪条件:萃取温度70 ℃,设置加热时间4 min,萃取压强:6 MPa,设置循环次数:3,淋洗体积60 %,氮吹时间60 s,开始萃取; 4. After completing step 3, set the conditions of the pressurized solvent extractor: extraction temperature 70 °C, set heating time 4 min, extraction pressure: 6 MPa, set cycle times: 3, rinse volume 60%, nitrogen blowing time 60 s, start extraction;

   5、萃取完成后,萃取液进入收集瓶,取出收集瓶,将萃取液过滤,真空浓缩至1/4体积,去除蛋白,反复操作,直至分界面无白色混悬为止,加入75 %-100 %乙醇,醇沉5~12 h,干燥得板栗多糖。 5. After the extraction is completed, the extract enters the collection bottle, take out the collection bottle, filter the extract, concentrate in vacuum to 1/4 volume, remove the protein, and repeat the operation until there is no white suspension at the interface, add 75%-100% ethanol, alcohol precipitation for 5-12 h, and drying to obtain chestnut polysaccharide.

  上述实施例仅用于作为本发明的技术方案的参考,不作为技术方案本身的单一限制条件。 The above-mentioned embodiments are only used as a reference for the technical solution of the present invention, and not as a single restriction of the technical solution itself.

Claims (3)

1.一种利用加压溶剂萃取方法提取板栗多糖的工艺,其特征在于,包括: 1. a process utilizing pressurized solvent extraction method to extract chestnut polysaccharide, is characterized in that, comprises:  (1)将板栗剥壳,取板栗仁烘干,温度为25℃-50℃,然后用粉碎机研磨成板栗粉,装入密封袋后,放入干燥器中,备用; (1) Shell the chestnuts, dry the chestnut kernels at a temperature of 25°C-50°C, then grind them into chestnut powder with a grinder, put them into a sealed bag, put them in a desiccator, and set aside;   (2)取上述处理的干燥板栗粉与硅藻土充分混合均匀,装入萃取池中,然后再加入1~20 kg硅藻土填满萃取池,连接好氮气装置、萃取仪和收集瓶; (2) Mix the above-mentioned dried chestnut powder with diatomaceous earth, put it into the extraction tank, then add 1~20 kg of diatomaceous earth to fill the extraction tank, and connect the nitrogen device, extraction instrument and collection bottle; (3)分别打开氮气和萃取仪开关,萃取仪自检,用清洗溶剂清洗萃取仪管道,设定预热温度开始预热; (3) Turn on the switch of nitrogen gas and extractor respectively, self-check the extractor, clean the pipeline of the extractor with cleaning solvent, set the preheating temperature and start preheating; (4)步骤3完成后,设置加压溶剂萃取仪条件:萃取温度50 ℃-70 ℃,设置加热时间4 min-20 min,萃取压强:3 MPa-15 MPa,设置循环次数:1-5次,淋洗体积40 %-60 %,氮吹时间40-100 s,开始萃取; (4) After step 3 is completed, set the conditions of the pressurized solvent extractor: extraction temperature 50 ℃-70 ℃, set heating time 4 min-20 min, extraction pressure: 3 MPa-15 MPa, set the number of cycles: 1-5 times , rinse volume 40%-60%, nitrogen blowing time 40-100 s, start extraction; (5) 萃取完成后,萃取液进入收集瓶,将萃取液过滤,真空浓缩至1/4体积,去除蛋白,反复操作,直至分界面无白色混悬为止,加入75 %-100 %乙醇,醇沉5~12 h,干燥得板栗多糖。 (5) After the extraction is completed, the extract enters the collection bottle, filters the extract, concentrates it in vacuum to 1/4 volume, removes the protein, and repeats the operation until there is no white suspension at the interface, then adds 75%-100% ethanol, alcohol Sink for 5-12 h, and dry to obtain chestnut polysaccharide. 2.根据权利要求1所述的提取板栗多糖的工艺,其特征在于,所述步骤(2)中的板栗粉与硅藻土按20 Kg  :10~30 Kg的比例混合。 2. The process for extracting chestnut polysaccharides according to claim 1, characterized in that, the chestnut powder in the step (2) is mixed with diatomaceous earth in a ratio of 20 Kg: 10-30 Kg. 3.根据权利要求1所述的提取板栗多糖的工艺,其特征在于,所述的清洗溶剂与萃取溶剂均为纯水。 3. the process for extracting chestnut polysaccharide according to claim 1, is characterized in that, described cleaning solvent and extraction solvent are pure water.
CN2012101637910A 2012-05-24 2012-05-24 Process for extracting chestnut polysaccharide by pressurized solvent extraction method Pending CN102702376A (en)

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CN103142721A (en) * 2013-03-15 2013-06-12 河北科技师范学院 Method for extracting triterpenoid from anli pear
CN104592412A (en) * 2015-02-28 2015-05-06 周可幸 Method for extracting chestnut polysaccharide
CN104861085A (en) * 2015-06-16 2015-08-26 河北大学 Chestnut seed alpha-1,6-glucan, preparation method for alpha-1,6-glucan, and application of alpha-1,6-glucan to anticancer drugs
CN105754001A (en) * 2016-04-26 2016-07-13 吉林化工学院 Method for extracting polysaccharides in polygonatum odoratum through solvent pressurizing method
CN107880147A (en) * 2017-12-26 2018-04-06 河北科技师范学院 Chinese chestnut active anticancer polysaccharide and its isolation and purification method
CN107982276A (en) * 2017-12-26 2018-05-04 河北科技师范学院 Purposes of the chestnut polysaccharide in the medicine for suppressing growth of cancer cells is prepared
CN109134690A (en) * 2018-11-12 2019-01-04 运城学院 A kind of ultrasonic wave auxiliary Polysaccharide in Pleurotus eryngii extraction process
CN114522926A (en) * 2022-02-18 2022-05-24 茶陵晶辉电子实业有限公司 Integral display screen cleaning equipment and cleaning method

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