Method for extracting rutin

Abstract

The present invention relates to the technical field of the preparation of plant extracts, and in particular to a method for extracting rutin. The method for extracting rutin involves extracting rutin by means of using Sophorae flos decoction pieces as a raw material, and comprises the step of mixing Sophorae flos decoction pieces with an extraction solvent for extraction, wherein the Sophorae flos decoction pieces are prepared by means of a method comprising the steps of: curing Sophorae flos, fermenting same, and then performing a cracking treatment to make cracks between petals of the Sophorae flos, wherein the mass proportion of fine powder obtained by means of passing the Sophorae flos decoction pieces through a 40-mesh sieve is not more than 25%. Compared with the traditional processing technology for Sophorae flos, the method for preparing Sophorae flos decoction pieces can effectively reduce the loss of rutin, and can significantly improve the leaching efficiency of rutin and reduce the leaching of impurity components such as polysaccharides. By means of the method for extracting rutin, the efficient extraction of rutin from Sophorae flos can be achieved, and the dissolution of impurity components during extraction can also be reduced, so that green and efficient industrial production of Sophorae flos-derived rutin can be achieved.

Description

A method for extracting rutin

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority to Chinese patent application number 202311115845.0, entitled "A Method for Extracting Rutin," filed with the Chinese Patent Office on August 31, 2023, the entire contents of which are incorporated herein by reference. Technical Field

[0003] The present invention relates to the technical field of plant extract preparation, in particular to a method for extracting rutin. Background Art

[0004] Sophora japonica (Sophora japonica L.) is the dried flower bud of the leguminous plant Sophora japonica, with a long history of medicinal use. China, the origin of this traditional Chinese medicine, is rich in resources. Rutin, the main active ingredient in Sophora japonica, has a variety of physiological activities, including maintaining and restoring the normal elasticity of capillaries, enhancing resistance, and preventing blood cell aggregation. With the continuous improvement of people's living standards and quality of life, the incidence of cardiovascular and cerebrovascular diseases is also on the rise, and its mortality rate ranks first among all diseases. Rutin and its derivatives have outstanding therapeutic effects on cardiovascular and cerebrovascular diseases and have been widely used in the clinical treatment of cardiovascular and cerebrovascular-related diseases in recent years. Rutin extraction has also become the most important industrial application of Sophora japonica.

[0005] The most common method for extracting rutin in industrial production and laboratories is alkaline extraction followed by acid precipitation. Borax is often added to stabilize the rutin in the system. This method consumes approximately 50 tons of water per ton of Sophora japonica seedlings. The excessive use of acid, alkali, and borax in the production process also causes severe environmental pollution. There are also reports on solvent extraction methods. CN201410071147.X discloses a green extraction process for rutin, a natural active flavonoid. The process involves crushing Sophora japonica seedlings to 40-60 mesh size, placing them in a tank, soaking them in 5-8 times diluted ethanol for 1 hour, and then stirring for 3-5 hours, for a total of three extraction cycles. After the extract is concentrated to remove most of the alcohol, stirring is continued for 1-2 hours to obtain crude rutin. The crude rutin is dissolved in 0.5% alkaline water, filtered, acidified, crystallized, filtered, and dried to obtain refined rutin. CN201310486906.4 discloses a preparation process of rutin, which comprises crushing the raw material into 60-120 mesh, heating with refined methanol and acid, boiling and refluxing for 1.5-3 hours, adding refined methanol and acid mixed solvent to the sophora japonica rice residue, adjusting the pH, and then adding calcium salt, heating, boiling and refluxing for 1-3 hours, filtering, washing the filter residue, concentrating the filtrate, adding water, adjusting the pH and crystallizing, washing with water of a certain pH, adding the methanol-spinning material again, pulping, centrifuging, drying, and crushing to obtain a rutin product with a content of 97-99%. CN201210237091.1 discloses a rutin extraction method, which comprises crushing the sophora japonica seed raw material to 50 mesh, adding 4 times, 3 times, and 3 times the amount of methanol to extract three times, with each reflux extraction time being 3 hours, 2 hours, and 2 hours respectively. The extract is concentrated until there is no methanol in the thick paste, and lime water and borax are added. After dissolving, filtering, acid adjustment, refiltration, and drying, pure rutin is obtained; the mother liquor is re-recovered with resin; the purity of the obtained rutin product is 98.69%. The above solvent extraction method first crushes the sophora japonica seed and then adds the extraction solvent for reflux extraction. In addition, alkali dissolution and acid precipitation are required in the extraction or refining process. In addition, the obtained crude rutin needs to be refined again to obtain high-content rutin.

[0006] Summary of the Invention

[0007] The invention provides a method for extracting rutin from sophora japonica seeds.

[0008] To better ensure the extraction efficiency of rutin, the prior art typically uses Sophora japonica seeds as raw materials for rutin extraction by crushing the seeds into a fine powder. However, using the crushed Sophora japonica seeds as raw materials causes polysaccharides and other components in the seeds to be leached during the subsequent extraction process, resulting in a decrease in the purity of rutin. This not only increases the difficulty of rutin purification and often requires multiple, complex refining steps to obtain a high-purity rutin product, but also results in waste and reduced content of polysaccharides and other components in the extracted residue. During the research and development process, the present invention unexpectedly discovered that, without the need to crush the sophora japonica seeds, the sophora japonica seeds can be subjected to ripening, proofing and cracking treatments (i.e., the sophora japonica seeds raw material is pre-treated by the above steps) so that the petals of the sophora japonica seeds are cracked; moreover, by controlling the amount of fine powder after the above treatment, while ensuring a high rutin extraction yield, the extraction of macromolecular components such as polysaccharides can be significantly reduced, thereby improving the purity of rutin, reducing the difficulty and complexity of subsequent refining, and retaining more macromolecules such as polysaccharides in the material residue after extraction for subsequent application; in addition, compared with the traditional sophora japonica seeds raw material processing method, the above processing method significantly reduces the loss of rutin during the processing process.

[0009] Specifically, the present invention provides the following technical solutions:

[0010] The present invention provides a method for extracting rutin, which uses Sophora japonica decoction pieces as raw materials to extract rutin, comprising the steps of mixing the Sophora japonica decoction pieces with an extraction solvent for extraction;

[0011] The sophora japonica flower slices are prepared by a method comprising the following steps: ripening the sophora japonica flower and then proofing it, and then cracking the sophora japonica flower petals to form cracks;

[0012] The mass proportion of the fine powder of the Sophora japonica flower slices that passes through a 40-mesh sieve is no more than 25%.

[0013] Preferably, the mass percentage of the fine powder of the Sophora japonica slices passing through a 40-mesh sieve is 5-25%. Controlling the mass percentage of the fine powder of the Sophora japonica slices within the above range can significantly improve the rutin extraction yield while retaining more macromolecular components such as polysaccharides in the extracted residue, thereby improving the utilization value of the residue.

[0014] In the medicinal slices obtained by the above medicinal slice preparation method, most of the Sophora japonica seeds still maintain relatively complete flower buds with cracks between the petals.

[0015] In the above method, the terminal temperature of the proofing is 50-70°C.

[0016] In the above method, the moisture content at the end point of proofing is 10-15%.

[0017] The endpoint temperature of the above-mentioned proofing refers to the temperature at the end of proofing, and the endpoint moisture content refers to the moisture content of the Sophora japonica rice at the end of proofing.

[0018] After the high temperature aging treatment, the sophora japonica seeds are directly subjected to a proofing treatment to the above-mentioned terminal temperature and moisture. The proofing treatment is to place the sophora japonica seeds after the aging treatment under certain temperature and humidity conditions until the terminal temperature and moisture of the proofing are reached.

[0019] The present invention does not impose any special restrictions on the equipment for proofing. Those skilled in the art can choose to perform proofing under cooling water and / or nitrogen flow conditions as needed, as long as the endpoint temperature and endpoint moisture of the proofing are reached.

[0020] The present invention finds that if the cracking treatment is directly performed without proofing after high-temperature aging, the viscosity of the sophora japonica seedlings will be large, making the cracking treatment difficult to perform. Furthermore, by controlling the terminal temperature and moisture content of the proofing within the above-mentioned range, the integrity of the sophora japonica seedlings after the cracking treatment can be significantly improved while ensuring the cracking effect (causing the petals to crack), and the amount of fine powder can be controlled within the above-mentioned required range, significantly reducing the leaching of macromolecular components such as polysaccharides, while being more conducive to ensuring the extraction efficiency of rutin.

[0021] In the above method, the cracking is performed by extrusion cracking.

[0022] Extrusion cracking refers to a method of opening the object to be processed by extrusion. There is no particular limitation on the equipment used for extrusion cracking in the present invention, and conventional extrusion cracking equipment can be used.

[0023] In some embodiments of the present invention, a double-roller machine is used for cracking treatment, and the hydraulic pressure of the double-roller machine is 2-4 MPa.

[0024] In the above method, the aging is high-temperature aging.

[0025] Preferably, the aging temperature is 90-140°C.

[0026] The aging time is 20 to 60 minutes.

[0027] Controlling the curing temperature and time within the above range is beneficial to reducing the loss of effective ingredients such as rutin during the processing process. Moreover, it can better ensure the integrity of the Sophora japonica seeds after cracking treatment and control the amount of fine powder within the above required range.

[0028] There is no particular limitation on the raw materials of Sophora japonica seeds for preparing Sophora japonica seeds slices in the present invention. Untreated freshly picked (dried) Sophora japonica seeds or properly stored (dried) Sophora japonica seeds can be used.

[0029] On the basis of the above-mentioned pretreatment method of Sophora japonica raw materials and in accordance with the characteristics of preparing Sophora japonica decoction pieces by the pretreatment method, the present invention further optimizes the extraction step of rutin.

[0030] Preferably, in the above rutin extraction method, the extraction solvent is 85%-95% methanol aqueous solution and / or 70%-80% ethanol aqueous solution.

[0031] Preferably, in the extraction, the mass volume ratio of the Sophora japonica pieces to the extraction solvent is 1 kg: (5-12) L.

[0032] Preferably, the extraction temperature is 55-70°C.

[0033] Preferably, the extraction method is continuous countercurrent.

[0034] Preferably, the extraction time is 1-10 hours.

[0035] The extraction of rutin can be carried out using conventional extraction equipment. There is no special restriction on the number of extractions. According to industrial needs, the number of extractions can be increased or a cyclic extraction method can be adopted.

[0036] In industrial applications, extraction can be carried out using tank groups, basket buckets, horizontal rotation, etc., and the produced liquid can be concentrated and crystallized.

[0037] The above-mentioned rutin extraction method further comprises: concentrating the extracted extract to 1 / 4.5-1 / 7.5 of the original volume and then crystallizing it.

[0038] Preferably, the crystallization is cooling stirring crystallization, the crystallization time is 5-10 hours, and the terminal temperature of the crystallization is 10-50°C.

[0039] Preferably, after crystallization, wet crystals are obtained by solid-liquid separation, and the extraction solvent is used to wash the wet crystals.

[0040] In the above wet crystal washing, the volume of the extraction solvent is 1-2 times the mass of the Sophora japonica flower slices.

[0041] The beneficial effects of the present invention are as follows: the present invention uses the sophora japonica flower slices as raw materials to extract rutin. Compared with the traditional sophora japonica flower processing technology, the preparation method of the sophora japonica flower slices adopted by the present invention can effectively reduce the loss of rutin and realize the retention of rutin in the sophora japonica flower to a greater extent; moreover, the sophora japonica flower slices prepared by the method can significantly improve the leaching efficiency of rutin, while reducing the leaching of impurity components such as polysaccharides, and retaining macromolecular components such as polysaccharides in the sophora japonica flower residue to a greater extent, so that the application value of the residue is maximized, and the comprehensive output and added value of the sophora japonica flower resources are improved.

[0042] The rutin extraction method provided by the present invention can realize the efficient extraction of rutin from sophora japonica buds, has a high rutin extraction yield, and simultaneously reduces the dissolution of impurity components in the extraction process, improves the refining efficiency of rutin, and realizes that a high-purity rutin product can be prepared with only simple refining (one-step concentration and crystallization). The use of acid and alkali in the rutin extraction process and the resulting environmental pollution problems are completely avoided. The process is simple and easy to implement, and can realize the green and efficient industrial production of rutin derived from sophora japonica buds. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 shows Sophora japonica seeds.

[0044] Figure 2 shows the Sophora japonica pieces prepared in this application.

[0045] Figure 3 is the detection spectrum.

[0046] Figure 4 is the standard curve. DETAILED DESCRIPTION

[0047] To make the objectives, technical solutions, and advantages of the present invention more clear, the technical solutions of the present invention are described clearly and completely below. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0048] According to the Pharmacopoeia (2020 edition):

[0049] This product is the dried flowers and buds of Sophora japonica L., a plant in the Leguminosae family. Harvested in summer when the flowers open or the buds form, they are promptly dried, and branches, stems, and impurities are removed. The former are commonly known as "sophora flowers," and the latter as "sophora rice."

[0050] Sophora japonica flowers are wrinkled and curled, with petals often scattered. The complete calyx is bell-shaped, yellow-green, and shallowly lobed at the apex. There are five petals, yellow or yellowish-white; one is larger, nearly round, and slightly concave at the apex; the other four are oblong. There are ten stamens, nine of which are fused at the base. The filaments are slender. The pistil is cylindrical and curved. The plant is light in weight, with a faint odor and a slightly bitter taste.

[0051] Sophora japonica: Oval or elliptical, 2-6 mm long and approximately 2 mm in diameter. The lower calyx has several longitudinal striations. Above the calyx are yellowish-white, unopened flowers. The pedicel is small. The plant is light and crumbles easily when touched. It has a faint odor and a slightly bitter taste. (See Figure 1).

[0052] The pharmacopoeia defines Sophora japonica as the dried flower buds of the leguminous plant Sophora japonica L. Drying can be done by air-drying or oven-drying. In practice, farmers harvest Sophora japonica, but due to equipment limitations, they often air-dry. Distributors then purchase them from farmers. The Sophora japonica mentioned in this application refers to dried Sophora japonica.

[0053] The Sophora japonica seeds used in the examples were purchased by the applicant from a dealer and were in the state of dried flower buds.

[0054] Sampling was carried out in accordance with the 2020 edition of the Chinese Pharmacopoeia, Part IV, General Chapter 0211; the determination of moisture in Sophora japonica rice was carried out in accordance with the 2020 edition of the Chinese Pharmacopoeia - the moisture determination method in Sophora japonica flower; the determination of rutin was shown in Appendix A.

[0055] The aging device used in the preparation method of the present invention can be a disc dryer, a degassing machine, an oven, a distillation pot, a wok or other device that can be uniformly heated, and the proofing device can be a disc dryer, a degassing machine, an oven, a distillation pot, a wok or other device that can uniformly control the temperature. It can be configured according to the equipment conditions of the workshop. If the equipment allows, the aging equipment can be considered for in-situ proofing. In order to eliminate the influence of different equipment on the amount of fine powder of the decoction pieces, all the following examples and comparative examples are carried out using the same aging and proofing equipment.

[0056] The equipment used in the embodiment is a degassing machine, specifically including a first-stage degassing machine and a second-stage degassing machine. By controlling the steam pressure and / or the rotation motor frequency of the degassing machine, a refrigerant is introduced into the jacket to control the temperature of the gas inside the equipment / or the material is placed under nitrogen flow conditions until the material or environment reaches the target temperature or moisture content requirements.

[0057] Example 1

[0058] This embodiment provides a method for preparing Sophora japonica slices, the steps of which are as follows:

[0059] 5t of raw Sophora japonica rice (the raw Sophora japonica rice was tested to have a rutin content of 19.98% and a moisture content of 13.0%) was transferred to a raw material bin through a feeding auger, and transported to a first-level evaporator for curing through a scraper. The curing temperature was 140°C and the curing time was 20min. Thereafter, the raw Sophora japonica rice was transferred to a second-level evaporator in a closed state through a feeding scraper for proofing (circulating water was introduced into the jacket). The final proofing temperature was 59-61°C, and the final proofing moisture was 13.0-13.5%. After proofing, the Sophora japonica rice was cracked by a roller machine so that cracks were formed between the petals of the Sophora japonica rice. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica rice slices. The mass of the fine powder passing through the 40-mesh sieve of the Sophora japonica rice slices was 10%.

[0060] The Sophora japonica pieces prepared in this application are shown in Figure 2.

[0061] Example 2

[0062] This embodiment provides a method for preparing Sophora japonica slices, the steps of which are as follows:

[0063] 5t of raw Sophora japonica rice (the raw Sophora japonica rice was tested to have a rutin content of 18.46% and a moisture content of 12.5%) was transferred to a raw material bin through a feeding auger, and transported to a first-level steam evaporator for ripening through a scraper. The ripening temperature was 90°C and the ripening time was 60min. Thereafter, the raw Sophora japonica rice was transferred to a second-level steam evaporator in a closed state through a feeding scraper for proofing. The proofing end temperature was 50-52°C, and the proofing end moisture was 14.5-15.0%. After proofing, the Sophora japonica rice was cracked by a roller machine so that cracks were formed between the petals of the Sophora japonica rice. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica rice slices. The mass of the fine powder passing through a 40-mesh sieve of the Sophora japonica rice slices accounted for 8%

[0064] Example 3

[0065] This embodiment provides a method for preparing Sophora japonica slices, the steps of which are as follows:

[0066] 5t of raw Sophora japonica seeds (the raw Sophora japonica seeds were tested to have a rutin content of 17.47% and a moisture content of 12.5%) were transferred to a raw material bin through a feeding auger, and transported to a first-level evaporator for ripening through a scraper. The ripening temperature was 130°C and the ripening time was 30min. Thereafter, the seeds were transferred to a second-level evaporator in a closed state through a feeding scraper for proofing. The proofing end temperature was 50-52°C, and the proofing end moisture was 10.0-10.5%. After proofing, the Sophora japonica seeds were cracked by a roller machine so that cracks were formed between the petals of the Sophora japonica seeds. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica seeds slices. The mass of the fine powder passing through a 40-mesh sieve of the Sophora japonica seeds slices was 25%.

[0067] Example 4

[0068] This embodiment provides a method for preparing Sophora japonica slices, the steps of which are as follows:

[0069] 5t of raw Sophora japonica seeds (the raw Sophora japonica seeds were tested to have a rutin content of 19.32% and a moisture content of 13.0%) were transferred to a raw material bin through a feeding auger, and transported to a first-level steam evaporator for ripening through a scraper. The ripening temperature was 110°C and the ripening time was 40min. Thereafter, the seeds were transferred to a second-level steam evaporator in a closed state through a feeding scraper for proofing. The proofing end temperature was 68-70°C, and the proofing end moisture was 10.0-10.5%. After proofing, the Sophora japonica seeds were cracked by a roller machine so that cracks were formed between the petals of the Sophora japonica seeds. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica seeds slices. The mass of the fine powder passing through a 40-mesh sieve of the Sophora japonica seeds slices accounted for 18%.

[0070] Example 5

[0071] This embodiment provides a method for preparing Sophora japonica slices, the steps of which are as follows:

[0072] 5t of raw Sophora japonica rice (the raw Sophora japonica rice was tested and the rutin content in the Sophora japonica rice was 20.41% and the moisture content was 13.0%) was transferred to the raw material warehouse through a feeding auger, and transported to a curing device through a scraper. The curing temperature was 105°C and the curing time was 50min. Thereafter, the Sophora japonica rice was transferred to a proofing device in a closed state. The proofing end temperature was 68-70°C, and the proofing end moisture was 14.5-15.0%. After proofing, the Sophora japonica rice was cracked by a roller machine so that cracks were formed between the petals of the Sophora japonica rice. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica rice slices. The mass of the fine powder of the Sophora japonica rice slices passing through a 40-mesh sieve accounted for 5%.

[0073] Example 6

[0074] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0075] The buds of Sophora japonica prepared by the method of Example 1 were used as raw materials for rutin extraction. 500 kg of the buds of Sophora japonica were transported to a 10 m 3 After the addition of materials to the extraction tank is completed, 5.0m 3 70% ethanol at 65-70℃, maintain 65-70℃, stir at 20Hz and extract for 1h, filter, extract 5 times under the same conditions, and obtain 24.5ml of extract 3 , stir each extraction liquid evenly, measure the volume, take samples, mix them according to proportion, and obtain the mixed extraction liquid.

[0076] Example 7

[0077] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0078] The buds of Sophora japonica prepared by the method of Example 2 were used as raw materials for rutin extraction. 500 kg of the buds of Sophora japonica were transported to a 10 m 3 After the addition of materials to the extraction tank is completed, 5.0m 3 70% ethanol at 65-70℃, maintain 65-70℃, stir at 20Hz and extract for 1h, filter, extract 5 times under the same conditions, and obtain 24.5ml of extract 3 , stir each extraction liquid evenly, measure the volume, take samples, mix them according to proportion, and obtain the mixed extraction liquid.

[0079] Example 8

[0080] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0081] The buds of Sophora japonica prepared by the method of Example 3 were used as raw materials for rutin extraction. 500 kg of the buds of Sophora japonica were transported to a 10 m 3 After the addition of materials to the extraction tank is completed, 5.0m 3 70% ethanol at 65-70℃, maintain 65-70℃, stir at 20Hz and extract for 1h, filter, extract 5 times under the same conditions, and obtain 24.5ml of extract 3 , stir each extraction liquid evenly, measure the volume, take samples, mix them according to proportion, and obtain the mixed extraction liquid.

[0082] Example 9

[0083] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0084] The buds of Sophora japonica prepared by the method of Example 4 were used as raw materials for rutin extraction. 500 kg of the buds of Sophora japonica were transported to a 10 m 3 After the extraction tank is filled, pump 5.0m 3 70% ethanol at 65-70℃, maintain 65-70℃, stir at 20Hz and extract for 1h, filter, extract 5 times under the same conditions, and obtain 24.5ml of extract 3 , stir each extraction liquid evenly, measure the volume, take samples, mix them according to proportion, and obtain the mixed extraction liquid.

[0085] Example 10

[0086] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0087] The buds of Sophora japonica prepared by the method of Example 5 were used as raw materials for rutin extraction. 500 kg of the buds of Sophora japonica were transported to a 10 m 3 After the addition of materials to the extraction tank is completed, 5.0m 3 70% ethanol at 65-70℃, maintain 65-70℃, stir at 20Hz and extract for 1h, filter, extract 5 times under the same conditions, and obtain 24.5ml of extract 3 , stir each extraction liquid evenly, measure the volume, take samples, mix them according to proportion, and obtain the mixed extraction liquid.

[0088] Comparative Example 1

[0089] This comparative example provides a preparation method of Sophora japonica slices, and the steps are as follows:

[0090] 5t of raw Sophora japonica rice (the raw Sophora japonica rice was tested and found to have a rutin content of 20.00% and a moisture content of 13.0%) was transferred to the raw material silo through a feeding auger. The Sophora japonica rice directly entered the roller machine from the silo to crack the petals of the Sophora japonica rice. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica rice slices. The mass of the fine powder passing through the 40-mesh sieve accounted for 65%.

[0091] Comparative Example 2

[0092] This comparative example provides a preparation method of Sophora japonica slices, and the steps are as follows:

[0093] 5t of raw Sophora japonica rice (the raw Sophora japonica rice was tested and found to have a rutin content of 20.00% and a moisture content of 13.0%) was transferred to the raw material bin through a feeding auger, and transported to a desiccant steamer for ripening through a scraper. The ripening temperature was 100°C and the ripening time was 50min. Afterwards, the rice was transferred to a roller machine in a closed state for cracking. The hydraulic pressure of the roller machine was 2.9±0.5MPa. The equipment made an abnormal noise and was forced to stop. A large amount of Sophora japonica rice stuck to the rollers.

[0094] Comparative Example 3

[0095] This comparative example provides a preparation method of Sophora japonica slices, and the steps are as follows:

[0096] 5t of raw Sophora japonica rice (the raw Sophora japonica rice was tested to have a rutin content of 20.00% and a moisture content of 13.0%) was transferred to a raw material bin through a feeding auger, and transported to a first-level steam evaporator for curing through a scraper. The curing temperature was 100°C and the curing time was 50min. Thereafter, the raw Sophora japonica rice was transferred to a second-level steam evaporator in a closed state through a feeding scraper for proofing. The proofing end temperature was 40-42°C, and the proofing end moisture was 13.0-13.5%. After proofing, the Sophora japonica rice was cracked by a roller machine so that cracks were formed between the petals of the Sophora japonica rice. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica rice slices. The mass of the fine powder passing through a 40-mesh sieve of the Sophora japonica rice slices was 45%.

[0097] This comparative example also provides a method for extracting rutin, which comprises the following steps:

[0098] The bud slices prepared by the preparation method of the bud slices of Sophora japonica in this comparative example were used as raw materials for rutin extraction. 500 kg of the bud slices of Sophora japonica were transported to a 10 m 3 After the addition of materials to the extraction tank is completed, 5.0m 3 70% ethanol at 65-70℃, maintain 65-70℃, stir at 20Hz and extract for 1h, filter, extract 5 times under the same conditions, and obtain 24.5ml of extract 3 , stir each extraction liquid evenly, measure the volume, take samples, mix them according to proportion, and obtain the mixed extraction liquid.

[0099] Comparative Example 4

[0100] This comparative example provides a preparation method of Sophora japonica slices, and the steps are as follows:

[0101] 5t of raw Sophora japonica rice (the raw Sophora japonica rice was tested to have a rutin content of 20.00% and a moisture content of 13.0%) was transferred to a raw material bin through a feeding auger, and transported to a first-level evaporator for curing through a scraper. The curing temperature was 100°C and the curing time was 50min. Thereafter, the raw Sophora japonica rice was transferred to a second-level evaporator in a closed state through a feeding scraper for proofing. The proofing end temperature was 59-61°C, and the proofing end moisture was 5.0-5.5%. After proofing, the Sophora japonica rice was cracked by a roller machine so that cracks were formed between the petals of the Sophora japonica rice. The hydraulic pressure of the roller machine was 2.9±0.5MPa to obtain Sophora japonica rice slices. The mass of the fine powder passing through a 40-mesh sieve of the Sophora japonica rice slices accounted for 65%.

[0102] Experimental Example 1 Detection of rutin content and water content in Sophora japonica slices

[0103] The sophora japonica slices prepared in Examples 1-5 and Comparative Examples 3 and 4 were sampled at different locations and mixed to test for rutin content and moisture content. The test results are shown in Table 1. The results show that the rutin content of the sophora japonica slices of Examples 1-5 remains at a level comparable to that of the sophora japonica raw material before processing, and the dry basis content of the sophora japonica after processing is also at the same level as before processing.

[0104] Table 1

[0105] Experimental Example 2: Rutin Extraction Efficiency Detection

[0106] The rutin extraction efficiency and the retention of macromolecular components such as polysaccharides in the slag of the rutin extraction methods of Examples 6-10 and Comparative Example 3 were tested as follows:

[0107] The remaining residue after extraction is evaporated to dryness in the original extraction tank. Determine the mass volume solid content of the extract (dry matter / volume*100%), dry matter extraction rate (extracted dry matter / raw material dry matter*100%) and rutin volume content. The extract is vacuum dried at below 70°C to obtain a crude rutin extract with a volatile matter of ≤7%, and the rutin dry basis HPLC content is detected. The residue is vacuum dried at below 70°C to obtain a volatile matter of ≤7%, and after drying, the rutin, polysaccharide and protein content of the residue is detected (converted to a 10% moisture residue content). The residue is dried using a disc dryer and the mass of the residue with a volatile matter of 10.0% is determined.

[0108] The method of extracting rutin after crushing the sophora japonica seeds commonly used in the prior art was used as a control. The only difference between the method and the rutin extraction method of Examples 6-10 was that the sophora japonica seeds slices were replaced with sophora japonica seeds powder with a 80-mesh pass rate of 100% and a rutin content of 19.98%, and the moisture content of the sophora japonica seeds powder was 13.10%.

[0109] The test results are shown in Table 2. As shown in Table 2, the extraction of rutin was carried out using the Flos Sophorae Pulvis decoction pieces of Example 1-5 as raw material, and the extraction efficiency of rutin was higher (rutin extraction yield, rutin dry basis HPLC content were both higher, and the rutin content of the slag was lower). Moreover, the loss of components such as polysaccharides, fiber, and protein in the slag was less, and the content of components such as polysaccharides, fiber, and protein in the slag was significantly improved (the dry matter extraction rate was low, and the crude fiber content, crude protein content, and volatile matter of 10.0% of the slag were all higher). The control group replaced the Flos Sophorae Pulvis decoction pieces with 80 mesh pass rates of 100%, resulting in a reduction in the extraction efficiency of rutin, and significantly reducing the content of polysaccharides, fiber, protein, etc. in the slag, and significantly reducing the slag quality. The mass of the fine powder passed through a 40-mesh sieve by the Flos Sophorae Pulvis decoction pieces of Comparative Example 3 was 45%, and the Flos Sophorae Pulvis decoction pieces of Comparative Example 3 were used as extraction raw materials, resulting in a reduction in the extraction efficiency of rutin, and significantly reducing the content of polysaccharides, fiber, protein, etc. in the slag, and significantly reducing the slag quality.

[0110] Table 2

[0111] Additional notes:

[0112] Mass volume solid content: the weight of dry matter in 100ml of extract, that is, g / 100ml, the unit is %, mainly used to calculate the dry matter extraction rate.

[0113] Dry matter extraction rate: The solids dissolved during the extraction process of 100g of Sophora japonica seeds or medicinal slices, mainly indicating that the total solids dissolved during the medicinal slices extraction process are less than those during the powder extraction process.

[0114] Rutin volume content: The concentration of rutin in the extract, used to calculate the yield of rutin in the extraction process.

[0115] The following examples provide a method for extracting rutin using Sophora japonica flower slices as raw material in industrial production equipment, and verify the performance and application potential of the rutin extraction method in industrial production practice.

[0116] Example 11

[0117] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0118] The sophora japonica slices prepared by the method of Example 5 were used as raw materials for rutin extraction. The sophora japonica slices were fed through a basket extractor scraper, the feeding rate was controlled to be 20±0.2 kg per hour, 94.5-95.0% methanol aqueous solution was used as the extraction solvent, the extraction solvent replenishment rate was 160±1.6 L / h, the extraction solvent temperature was 55.0-55.5°C, the extractor operating frequency was adjusted to control the total extraction time to be 3.0-3.5 h, and the rutin extraction yield was calculated according to the amount of raw materials added per hour, the extracted extract, and the residual rutin in the slag after the extraction was completed.

[0119] The extract is concentrated using a thin film evaporator, the material temperature is controlled at 55-70°C, the vacuum degree is -0.050 to -0.095 MPa, and after being concentrated to 1 / 4.5 of the original volume, it is transferred to a crystallization tank for uniform cooling and stirring crystallization. The total crystallization time is 5 hours, the crystallization end temperature is 50°C, and the filter cake is rinsed with the extraction solvent. The rinse liquid is returned to the second-to-last extraction process of the extractor, and the filter cake is vacuum dried to obtain the rutin product.

[0120] The extraction yield of rutin was calculated as follows: (weight of rutin produced daily × HPLC content) / weight of Sophora japonica flower slices input daily × HPLC content). After the production system was stabilized, the extraction yield of rutin was calculated to be 92.3%, and the dry basis content of the rutin product was 98.5% (HPLC).

[0121] Example 12

[0122] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0123] The buds of sophora japonica prepared by the method of Example 5 were used as raw materials for rutin extraction, and the buds of sophora japonica were transported to a 10m3 slurry container for extraction by a scraper. 3In a horizontal extraction tank, 1 ton of Sophora japonica slices was added to each tank, and 7000L of 90.0-90.5% methanol aqueous solution (volume fraction) was pumped in as an extraction solvent. The extraction solvent was heated to 60-60.5°C by a heat exchanger, and the temperature in the tank was maintained at 59-61°C. The first pot was extracted 5 times with the extraction solvent, each extraction lasting 0.75-1.0h. From the second pot onwards, the extraction solvent was supplemented only in the last extraction. The 2nd, 3rd, 4th, and 5th extracts of the previous pot were used for the 1st, 2nd, 3rd, and 4th extractions of the current pot, respectively. Only the extract of the first extraction of the raw material was extracted and entered the concentration process. From the 5th pot onwards, the extract was concentrated using a thin film evaporator, the material temperature was controlled at 55-70°C, the vacuum degree was -0.050 to -0.095 MPa, and after being concentrated to 1 / 6 of the original volume, it was transferred to a crystallization tank for uniform cooling and stirring crystallization. The total crystallization time was 7.5 hours, the crystallization endpoint temperature was 30°C, and the filter cake was rinsed with 3.0 times the amount (m / v) of the wet filter cake of the extraction solvent. The rinsing liquid was returned to the 4th-stage extraction tank extraction process, and the filter cake was vacuum dried to obtain the rutin product.

[0124] After the production system is stabilized, the rutin extraction yield is calculated using the formula: rutin extraction yield = (weight of rutin produced per pot × rutin HPLC content of the product) / (weight of the corresponding pot of Sophora japonica slices × rutin HPLC content of the product). The calculated rutin extraction yield is 96.5%, and the dry basis content of the rutin product is 95.6% (HPLC).

[0125] Example 13

[0126] This embodiment provides a method for extracting rutin, which comprises the following steps:

[0127] The sophora japonica slices prepared by the method of Example 5 were used as raw materials for rutin extraction. The sophora japonica slices were fed through the scraper of a horizontal rotary extractor, the feeding rate was controlled to be 1000 ± 20 kg per hour, 85.0-85.5% methanol aqueous solution was used as the extraction solvent, the replenishment rate of the extraction solvent was 10000 ± 100 L / h, the extraction solvent temperature was 63.5-64.0 ° C, the extractor operating frequency was adjusted and the total extraction time was controlled to 6-7 h. After running for 7 h, the rutin extraction yield was calculated according to the amount of raw materials added per hour, the extracted extract, and the residual rutin in the slag.

[0128] The extract is concentrated using a thin film evaporator, the material temperature is controlled at 55-70°C, the vacuum degree is -0.050 to -0.095 MPa, and the extract is concentrated to 1 / 7.5 of the original volume and then transferred to a crystallization tank for uniform cooling and stirring crystallization. The total crystallization time is 10 hours, the crystallization end temperature is 10°C, and the filter cake is filtered. The filter cake is rinsed with 4.5 times the amount (m / v) of the extraction solvent as the wet filter cake. The rinse liquid is returned to the penultimate extraction process of the extractor, and the filter cake is vacuum dried to obtain the rutin product.

[0129] After the production system stabilized, the rutin extraction yield was calculated using the formula: rutin extraction yield = (weight of rutin produced daily × HPLC content) / weight of Sophora japonica flower slices put in daily × content). The calculated rutin extraction yield was 97.8%, and the dry basis content of the rutin product was 93.2% (HPLC).

[0130] Appendix A

[0131] Inspection methods

[0132] A.1 General Provisions

[0133] Unless otherwise specified, the reagents and water used in this standard refer to analytically pure reagents and grade 3 water specified in GB / T 6682-2008.

[0134] A.2 Instruments and Equipment

[0135] A.2.2.1 High performance liquid chromatograph equipped with UV-visible detector;

[0136] A.2.2.2 Ultrasonic cleaner;

[0137] A.2.2.3 Analytical balance (sensitivity 0.0001g);

[0138] A.3 Detection steps

[0139] A.3.3.1 Preparation of standard samples

[0140] A.3.3.1.1 Standard stock solution: Weigh about 10 mg of the standard substance and place it in the same 25 mL brown volumetric flask. Dissolve it with chromatographic methanol by ultrasonication and then adjust the volume. Transfer it to a special standard solution bottle as the stock solution and store it in a refrigerator at 4°C. The validity period is one year.

[0141] A.3.3.1.2 Standard curve: dilute the mixed stock solution with methanol in equal multiples to obtain 5 concentration levels, draw a standard curve, and determine the linear range.

[0142] A.3.3.1.3 Standard working solution: Dilute the standard stock solution to a concentration of approximately 0.1 mg / mL and place it in a dedicated standard solution bottle as the working solution. Store in a refrigerator at 4°C and the validity period is one year.

[0143] A.3.3.2 Preparation of sample solution

[0144] A.3.3.2.1 Powder sample: weigh approximately 0.5000 g of sample in parallel and place in a 50 mL volumetric flask. Add methanol and sonicate to dissolve the sample. Cool, adjust to volume, and mix thoroughly for testing.

[0145] A.3.3.2.2 Liquid sample: Weigh or pipette a certain amount of sample, dilute it with methanol by a certain multiple, mix well and then test.

[0146] A.3.3.3 Reference liquid chromatography conditions

[0147] A.3.3.3.1 Chromatographic column: 48#, C 18 Column (4.6 x 250 mm, 5 μm).

[0148] A.3.3.3.2 Chromatographic column temperature: 40℃.

[0149] A.3.3.3.3 Injection volume: 10μL.

[0150] A.3.3.3.4 Running time: 40 minutes.

[0151] A.3.3.3.5 Mobile phase conditions: acetonitrile: water: phosphoric acid = 190:810:8 (volume ratio).

[0152] A.3.3.3.6 Flow rate: 1.0 mL / min.

[0153] A.3.3.3.7 Wavelength: 360nm

[0154] A.3.3.4 See Figure 3 for the detection spectrum.

[0155] A.3.3.5 Result calculation

[0156] The external standard method was used for quantification, and the single point quantitative method was used for quantitative detection. The content of rutin in the sample was expressed as % as follows:

[0157] X=(S 样品 / S 标样 *C 标样 *K) / M 样品 / 10

[0158] Where: X——the content of rutin in the sample, in %;

[0159] S sample - the peak area of ​​the sample detected on liquid chromatography;

[0160] S standard sample - the peak area of ​​the standard sample detected on the liquid chromatography;

[0161] C Standard - the concentration of the standard, in mg / mL;

[0162] K——sample dilution multiple;

[0163] Msample – the mass of the sample in g.

[0164] The calculation results are rounded to two decimal places. Powder samples are tested in parallel, with a parallelism error of 3% and a retest error of 5%.

[0165] Appendix: Accuracy Verification Data

[0166] 1. Drawing of standard curve for rutin quantification

[0167] 1.1 Preparation of Rutin Stock Solution:

[0168] Accurately weigh 0.21306 g of rutin reference substance, dilute to 100 mL with methanol, and filter through a 0.45 μm filter membrane.

[0169] 1.2 Drawing of the standard curve

[0170] The measurement data are shown in Table 3, and the standard curve is shown in Figure 4.

[0171] Table 3

[0172] Accurately measure the rutin stock solution and draw a standard curve based on the main peak area of ​​rutin and the concentration of the reference solution. 2 =0.999948.

[0173] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims

1. A method for extracting rutin, characterized in that: The method uses the Sophora japonica flower pieces as raw materials to extract rutin, comprising the steps of mixing the Sophora japonica flower pieces with an extraction solvent for extraction; The sophora japonica flower slices are prepared by a method comprising the following steps: ripening the sophora japonica flower, allowing it to ferment, and then performing a cracking treatment to cause cracks to form between the petals of the sophora japonica flower; The mass percentage of fine powder of the Sophora japonica root slices that passes through a 40-mesh sieve is no higher than 25%.

2. The method for extracting rutin according to claim 1, characterized in that The mass percentage of the fine powder of the Sophora japonica flower pieces passing through a 40-mesh sieve is 5-25%.

3. The method for extracting rutin according to claim 1 or 2, characterized in that The end point temperature of the proofing is 50-70°C; And / or, the moisture content at the end point of the proofing is 10-15%.

4. The method for extracting rutin according to any one of claims 1 to 3, characterized in that: The cracking is performed by extrusion cracking.

5. The method for extracting rutin according to any one of claims 1 to 4, characterized in that: The aging temperature is 90-140°C; Preferably, the aging time is 20 to 60 minutes.

6. The method for extracting rutin according to any one of claims 1 to 5, characterized in that: The extraction solvent is 85%-95% methanol aqueous solution and / or 70%-80% ethanol aqueous solution; Preferably, in the extraction, the mass volume ratio of the Sophora japonica pieces to the extraction solvent is 1 kg: (5-12) L.

7. The method for extracting rutin according to claim 6, characterized in that The extraction temperature is 55-70°C.

8. The method for extracting rutin according to any one of claims 6 to 7, characterized in that: The method further comprises: concentrating the extracted solution to 1 / 4.5-1 / 7.5 of the original volume and then crystallizing it.

9. The method for extracting rutin according to claim 8, characterized in that The crystallization is cooling stirring crystallization, the crystallization time is 5-10h, and the terminal temperature of the crystallization is 10-50°C.

10. The method for extracting rutin according to claim 8 or 9, characterized in that: After crystallization, wet crystals are obtained through solid-liquid separation, and the wet crystals are washed with the extraction solvent.

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