Disclosure of Invention
The invention overcomes the defects of the prior art, and discloses a method for extracting the rutin of tartary buckwheat. So as to improve the utilization rate of the tartary buckwheat and the purity of rutin.
In order to achieve the above purpose, the present invention is realized by the following technical scheme.
The extraction method of the tartary buckwheat rutin is characterized by comprising the following steps of:
1) Quick-freezing the fresh tartary buckwheat seeds.
2) Carrying out ultrasonic treatment on the quick-frozen tartary buckwheat seeds at the temperature ranging from-5 ℃ to-18 ℃; the frequency of ultrasonic vibration is 10KHz-20KHz, and the power is 1-3KW; the time of ultrasonic vibration is 10-40s.
3) Adding the ultrasonic-treated tartary buckwheat seeds into water, and boiling for 30-60min; and then cooling the water decoction to separate out crude rutin.
4) And recrystallizing the crude rutin with hot water to obtain a rutin finished product.
Preferably, the quick-freezing treatment is to make the center temperature of the fresh tartary buckwheat seeds reach-15 ℃ to-18 ℃ within 10 min.
Preferably, the ultrasonic treatment is to embed the vibrator of the ultrasonic device into the tartary buckwheat grains.
Preferably, the vibrator is cooled to-5 ℃ to-10 ℃.
Preferably, the time of the ultrasonic vibration is 30s.
Preferably, in the step 3), the boiled liquid is cooled to 10-20 ℃ and kept stand for 12-24 hours, and crude rutin is separated out.
Preferably, in the step 4), the crude rutin is dissolved by hot water at 98 ℃, filtered while the crude rutin is hot, naturally cooled to room temperature, and left to stand for crystallization, thus obtaining the rutin.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, fresh tartary buckwheat seeds are frozen in a quick-freezing mode, water in the tartary buckwheat seeds forms fine ice crystals, ultrasonic low-temperature treatment is adopted in the state, and acoustic flow and cavitation effect are generated in the tartary buckwheat seeds, so that the ice crystals form uniform and fine crystal grains, and the tartary buckwheat rutin is more easily released from the constraint of macromolecular substances under the action of the crystal grains; then through the steps of boiling water extraction and recrystallization, rutin components can be effectively extracted.
The invention does not use organic matters or acid-base solution for extraction, avoids the subsequent treatment steps, reduces the content of other substances in the rutin, effectively improves the purity of the rutin, and is simpler and more convenient in extraction method and beneficial to industrial production.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail by combining the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. The following describes the technical scheme of the present invention in detail with reference to examples, but the scope of protection is not limited thereto.
Example 1
A method for extracting rutin from Fagopyrum tataricum comprises the following specific steps:
1) 100g of fresh tartary buckwheat seeds which are newly harvested and full are cleaned and dried, and then quick-freezing treatment is carried out on the fresh tartary buckwheat seeds: the quick-freezing treatment is to make the center temperature of the fresh tartary buckwheat seeds reach-15 ℃ to-18 ℃ within 10 min.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat seeds at the temperature of-5 ℃; the frequency of ultrasonic vibration is 10KHz, and the power is 3KW; the time of ultrasonic vibration was 20s. The ultrasonic treatment is specifically carried out by cooling vibrator of ultrasonic device to-5deg.C, and then burying into fresh semen Fagopyri Tatarici.
3) Directly adding the fresh tartary buckwheat seeds subjected to ultrasonic treatment into cold water, and boiling for 30min; and then cooling the water decoction to 10 ℃ and standing for 24 hours to separate out crude rutin.
4) Dissolving crude rutin with 98deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
The high performance liquid chromatography external standard method is adopted to detect, and the mass content of rutin in the rutin refined product obtained by the embodiment is 96.9%.
Example 2
A method for extracting rutin from Fagopyrum tataricum comprises the following specific steps:
1) 100g of fresh tartary buckwheat seeds which are newly harvested and full are cleaned and dried, and then quick-freezing treatment is carried out on the fresh tartary buckwheat seeds: the quick-freezing treatment is to make the center temperature of the fresh tartary buckwheat seeds reach-15 ℃ to-18 ℃ within 10 min.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat seeds at the temperature of-18 ℃; the frequency of ultrasonic vibration is 20KHz, and the power is 2KW; the time of ultrasonic vibration was 30s. The ultrasonic treatment is specifically carried out by cooling vibrator of ultrasonic device to-10deg.C, and then burying into fresh semen Fagopyri Tatarici.
3) Directly adding the fresh tartary buckwheat seeds subjected to ultrasonic treatment into cold water, and boiling for 60 minutes; and then cooling the water decoction to 20 ℃ and standing for 24 hours to separate out crude rutin.
4) Dissolving crude rutin with 98deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
The high performance liquid chromatography external standard method is adopted to detect, and the mass content of rutin in the rutin refined product obtained by the embodiment is 98.7%.
Example 3
A method for extracting rutin from Fagopyrum tataricum comprises the following specific steps:
1) 100g of fresh tartary buckwheat seeds which are newly harvested and full are cleaned and dried, and then quick-freezing treatment is carried out on the fresh tartary buckwheat seeds: the quick-freezing treatment is to make the center temperature of the fresh tartary buckwheat seeds reach-18 ℃ within 10 min.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat seeds at the temperature of-10 ℃; the frequency of ultrasonic vibration is 20KHz, and the power is 1KW; the time of ultrasonic vibration was 40s. The ultrasonic treatment is specifically carried out by cooling vibrator of ultrasonic device to-10deg.C, and then burying into fresh semen Fagopyri Tatarici.
3) Directly adding the fresh tartary buckwheat seeds subjected to ultrasonic treatment into cold water, and boiling for 40min; and then cooling the water decoction to 20 ℃ and standing for 24 hours to separate out crude rutin.
4) Dissolving crude rutin with 98deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
The high performance liquid chromatography external standard method is adopted to detect, and the mass content of rutin in the rutin refined product obtained by the embodiment is 97.1%.
Example 4
A method for extracting rutin from Fagopyrum tataricum comprises the following specific steps:
1) 100g of fresh tartary buckwheat seeds which are newly harvested and full are cleaned and dried, and then quick-freezing treatment is carried out on the fresh tartary buckwheat seeds: the quick-freezing treatment is to make the center temperature of the fresh tartary buckwheat seeds reach-15 ℃ within 10 min.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains under the environment condition of-10 ℃; the frequency of ultrasonic vibration is 10KHz, and the power is 3KW; the time of ultrasonic vibration was 30s. The ultrasonic treatment is specifically carried out by cooling vibrator of ultrasonic device to-10deg.C, and then burying into fresh semen Fagopyri Tatarici.
3) Directly adding the fresh tartary buckwheat seeds subjected to ultrasonic treatment into cold water, and boiling for 40min; and then cooling the water decoction to 20 ℃ and standing for 24 hours to separate out crude rutin.
4) Dissolving crude rutin with 98deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
The high performance liquid chromatography external standard method is adopted to detect, and the mass content of rutin in the rutin refined product obtained by the embodiment is 98.2%.
Example 5
A method for extracting rutin from Fagopyrum tataricum comprises the following specific steps:
1) 100g of fresh tartary buckwheat seeds which are newly harvested and full are cleaned and dried, and then quick-freezing treatment is carried out on the fresh tartary buckwheat seeds: the quick-freezing treatment is to make the center temperature of the fresh tartary buckwheat seeds reach-15 ℃ within 10 min.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains under the environment condition of-18 ℃; the frequency of ultrasonic vibration is 10KHz, and the power is 2KW; the time of ultrasonic vibration was 40s. The ultrasonic treatment is specifically carried out by cooling vibrator of ultrasonic device to-10deg.C, and then burying into fresh semen Fagopyri Tatarici.
3) Directly adding the fresh tartary buckwheat seeds subjected to ultrasonic treatment into cold water, and boiling for 60 minutes; and then cooling the water decoction to 10 ℃ and standing for 24 hours to separate out crude rutin.
4) Dissolving crude rutin with 98deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
The high performance liquid chromatography external standard method is adopted to detect, and the mass content of rutin in the rutin refined product obtained by the embodiment is 97.6%.
Comparative example 1
100G of complete fresh tartary buckwheat seeds are selected and cleaned, then the cleaned tartary buckwheat seeds are put into clear water and soaked for 2-24 hours at the temperature of 10-50 ℃, the tartary buckwheat seeds are drained after the soaking is finished, then the drained tartary buckwheat seeds are dried in the environment with the temperature of 105 ℃, lime water with the pH value of 8-9 de is added, the leaching is carried out for different times under the condition of ultrasonic constant temperature leaching at the temperature of 80 ℃, and the leaching yield of rutin is measured.
The quality content of rutin in the rutin refined product obtained in comparative example 1 is 85.1% by detection with an external standard method of high performance liquid chromatography.
Comparative example 2
Crushing 100g of tartary buckwheat seeds to a particle size of 2mm, adding 2000g of calcium hydroxide aqueous solution, stirring and extracting for 5 hours, filtering, adjusting the pH value of the filtrate to 6.0 by using hydrochloric acid solution with the mass concentration of 5%, and then ultrafiltering to obtain ultrafiltrate; eluting the obtained ultrafiltration membrane filtrate with a chromatographic column, collecting eluent, concentrating and drying to obtain crude rutin, dissolving the crude rutin with 75g of hot water at 98 ℃, filtering while the crude rutin is hot, naturally cooling to room temperature, standing for crystallization for 12h, suction filtering, and drying to obtain rutin.
The quality content of rutin in the refined rutin product obtained in comparative example 2 is 89.2% by detection with an external standard method of high performance liquid chromatography.
Comparative example 3
Soaking 100g of fresh tartary buckwheat seeds in 50 ℃ water for 24 hours, and boiling for 40 minutes; and then cooling the water decoction to 20 ℃ and standing for 24 hours to separate out crude rutin. Dissolving crude rutin with 98deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
The high performance liquid chromatography external standard method is adopted to detect, and the mass content of rutin in the rutin refined product obtained in the comparative example 3 is 70.5%.
While the invention has been described in detail in connection with specific preferred embodiments thereof, it is not to be construed as limited thereto, but rather as a result of a simple deduction or substitution by a person having ordinary skill in the art to which the invention pertains without departing from the scope of the invention defined by the appended claims.