CN101461874A - Ultrasonic auxiliary method for simultaneously extracting areca alkaloids and coloring matter from betel nut - Google Patents

Abstract

The invention discloses a method for simultaneously extracting areca alkaloid and pigment from areca by an ultrasonic assisted method. The method comprises a pretreatment process of raw materials, a preparation process of extract, an extraction process of alkaloid and an extraction process of pigment. The method has simple technical process and can quickly extract areca alkaloid and pigment from areca at high efficiency with energy saving; moreover, the obtained areca pigment has better solubility and stability; therefore, the ultrasonic assisted method solves the problems that the domestic areca deep processing industry is laggard, the comprehensive utilization rate of areca active ingredients is low, and the like, thereby promoting the development of the domestic areca industry.

Description

Simultaneous extraction of betel nut alkaloids and pigments from betel nut by ultrasonic-assisted method

technical field

The invention relates to a method for simultaneously extracting betel nut alkaloids and pigments, in particular to a technology for preparing areca nut alkaloids and pigments with areca nuts as raw materials, and belongs to the technical field of postharvest processing of agricultural products.

Background technique

Areca nut (Arca catectu L.) is a precious tropical plant of the palm family with high economic value. The whole body of betel nut is a treasure, and its seeds, peel, flowers, and buds can be used as medicine. The commercial product of the seeds is called Langyu, which is a good astringent; Raw material of textile industry, after processing, can be made into high-quality fiber partitions and black dyes; tree trunks are used as building materials; complete dried fruit products are called dried nuts, which are chewed by people in Yunnan, Hainan, Taiwan, Hunan and other regions. Betel nut contains 0.3-0.6% alkaloids, 15% condensed tannin, 14% fat and areca red pigment. Among them, the alkaloids are mainly arecoline, with a content of 0.1-0.5%, and the rest are arecoline, desmethylarecoline, demethylarecoline, arecaline, homoarecoline, etc. In addition, betel nut endosperm contains catechins, anthocyanins and their polymers. The content of lauric acid, myristic acid and palmitic acid in betel nut oil is 78.4%, and unsaturated fatty acids such as oleic acid and linoleic acid account for about 19.1%. Among the free amino acids contained in betel nut, proline exceeds 15%, and tyrosine, phenylalanine and arginine exceed 10%. The medicinal value of betel nut is very high, ranking first among the "four major southern medicines". It is recorded in "Compendium of Materia Medica" that betel nut has many effects such as "lowering edema, clearing joints, invigorating the spleen, regulating the middle, and treating heartache accumulation". Betel nut also has the functions of treating glaucoma, increasing blood pressure, stopping diarrhea and treating dysentery, reducing inflammation and swelling, eliminating phlegm and asthma, purging qi and water, killing insects and removing accumulation. Modern medicine shows that the main effect of betel nut is reflected by the efficacy of arecoline. Arecoline (C ₈ H ₁₃ NO ₂ , mw.155) can excite M-choline receptors, which can cause increased secretion of glands, especially saliva secretion, and can also excite N-choline receptors, manifested as excitatory bone Muscle, ganglion and carotid body, etc., also have cholinergic effects on the central nervous system. In addition, arecoline can enhance gastrointestinal motility and cause diarrhea, so it can be taken to deworm; arecoline also has physiological functions such as constricting bronchi and causing vasodilation. Judging the quality of betel nut is mainly based on the content of arecoline and the quality of fiber.

Food coloring is the main component of food additives and is widely used in the pharmaceutical and cosmetic industries. Synthetic pigments are limited in use due to their low safety, while natural pigments are receiving more and more attention. Betel nuts contain a certain amount of pigment, and people have used betel nuts to make black fuel long ago. At present, the research reports on areca nut at home and abroad mainly focus on arecoline, catechin and other substances, and the utilization of areca nut is mainly the original product and primary processed product of areca nut, while the research on other active ingredients such as areca nut pigment, areca nut oil and betel nut protein Research reports are scarce. Hainan Province is the main betel nut planting base in my country, accounting for more than 95% of the country's total area and output. In 2006, Hainan's betel nut planting area was 796,000 mu, with a total output of 74,800 tons and an output value of about 1.2 billion yuan. However, the development of Hainan's betel nut deep-processing industry is seriously lagging behind. The main reason is that the betel nut is processed into dried betel nut and sold to the mainland. The added value of the product is low, and the comprehensive economic benefits of the industry are poor. If the active components such as alkaloids and pigments in betel nut are intensively processed and comprehensively utilized, it will effectively promote the development of my country's betel nut industry.

At present, there are many reports on the extraction methods of areca nut alkaloids, but mainly using organic solvents for extraction, which consumes a lot of reagents, takes a long time, and has a low extraction rate. However, there is no report on the simultaneous extraction and separation of arecoline and pigments assisted by ultrasound. Ultrasonic-assisted extraction is a relatively new type of extraction technology. The cavitation effect and secondary effect of ultrasonic waves can increase the permeability of cell membranes, and can accelerate the leaching and diffusion release of active ingredients in plants, thereby improving the extraction rate of active ingredients in plants and animals. . Therefore, the simultaneous extraction of areca nut alkaloids and areca nut pigments by ultrasonic-assisted method can not only shorten the production cycle, reduce the amount of solvent used, improve the extraction rate, but also help to realize the comprehensive utilization and deep processing of areca nut, and promote the rapid development of my country's areca nut industry .

Contents of the invention

The purpose of the present invention is to provide a method for simultaneously extracting areca alkaloids and pigments from betel nuts by ultrasonic-assisted method. Alkali and pigments are not only beneficial to the deep processing and comprehensive utilization of betel nuts, but also can promote the development of my country's betel nut industry.

Principle of the present invention is as follows:

Ultrasound refers to sound waves whose vibration frequency is greater than 20 kHz, and whose vibration frequency (frequency) per second is very high, exceeding the upper limit of human hearing (20000 Hz). Ultrasound has been widely used in the pharmaceutical industry, electromechanical industry, textile industry, chemical industry, food industry and other fields. Ultrasound has a series of mechanical, thermal, electromagnetic and chemical ultrasonic effects, such as mechanical effects, cavitation effects, thermal effects and chemical effects. Among them, the cavitation effect of ultrasonic waves accelerates the leaching of active ingredients in plants, and its secondary effects such as mechanical vibration, emulsification, diffusion, crushing, and chemical effects can also accelerate the diffusion and release of active ingredients. In addition, ultrasonic waves also have additional effects such as turbulent effects, perturbation effects, interface effects, and energy-gathering effects. These effects allow ultrasonic waves to not only shorten the extraction time and save the amount of solvent used when extracting the active components of the substance, but also improve the quality of some products. Therefore, the use of ultrasonic-assisted extraction technology can extract betel nut alkaloids and pigments from betel nuts in a relatively fast, efficient and energy-saving manner.

The present invention adopts for solving the technical solution of its technical solution:

A method for simultaneously extracting betel nut alkaloids and pigments from betel nuts by an ultrasonic-assisted method, comprising a raw material pretreatment process, an extract preparation process, an alkaloid extraction process, and a pigment extraction process, the steps of which are as follows:

1. Raw material pre-treatment process Select mature betel nut fruit, wash, remove green clothes, remove endogerm, then shred, dry, and crush to obtain betel nut powder.

2. Extraction preparation process Add ammonia water and anhydrous ether to betel nut powder at a ratio of 1:1 and 1:10~1:15 according to the ratio of mass/volume, and then use ultrasonic treatment for 30~60min; filter , collect the filtrate, and concentrate the filtrate to an extract.

3. Alkaloid extraction process Add an acidic solution to the above extract, filter it after fully dissolving, and collect the filtrate; adjust the pH of the filtrate to 7.0 with ammonia water, then add chloroform for extraction to obtain the extract; concentrate under reduced pressure and dry to obtain the betel nut biological alkali. The acidic solution is hydrochloric acid.

4. Pigment extraction process Take the filter residue obtained in step 2, add acidic ethanol solution at a ratio of 1:20 to 1:30 according to the mass/volume ratio, ultrasonically treat for 30 to 60 minutes, and then extract in a constant temperature water bath at 50 to 70°C; The extract is filtered, and then the filtrate is concentrated under reduced pressure until concentrated into an extract, and then dried to obtain the areca nut pigment. The acidic ethanol solution is 50% ethanol with HCl added.

Tests show that, when extracting at the same time for 2 hours, the ultrasonic-assisted method can increase the extraction rate of arecoline by 15.6% to 20.1% and the extraction rate of pigment by 33.8% to 49.1% compared with the common solvent extraction method. The test also shows that the obtained betel nut pigment is easily soluble in polar solvents such as water, ethanol, and ethanol solution, but insoluble in ether and petroleum ether. Moreover, the pigment has good heat resistance and light resistance. It has good stability in C, but poor stability in H ₂ O ₂ solution, and the wavelength scanning shows that it has a maximum absorption peak at 305nm.

Detailed ways

The present invention will be further illustrated below with non-limiting examples.

Embodiment one

1. Raw material pretreatment process Select mature betel nut fruit, wash, remove the green clothes, remove the betel nut inner germ, then shred, dry at 45°C, crush the dried betel nut, and pass through a 60-mesh sieve to obtain betel nut powder.

2. Extraction preparation process According to the mass/volume ratio, add ammonia water and anhydrous ether to the betel nut powder at a ratio of 1:1 and 1:10 respectively, and then use ultrasonic treatment for 30 minutes (frequency 28kHz, temperature 35°C) ; Filtrate, collect the filtrate, and concentrate the filtrate to extract.

3. Alkaloid extraction process Add 5 times the volume of 0.1mol/L HCl to the above extract, fully dissolve, filter, and collect the filtrate; adjust the pH of the filtrate to 7.0 with ammonia water, and then add it in a ratio of 1:10 (v/v) Chloroform, repeated extraction three times, combined chloroform extracts; concentrated under reduced pressure, dried to obtain areca nut alkaloids.

4. Pigment extraction process Take the filter residue obtained in step 2, add 50% ethanol solution containing 0.1mol/L HCl at a ratio of 1:25 according to the mass/volume ratio, and ultrasonically treat for 60 minutes (frequency 28kHz, temperature 35°C), and then Extract in a constant temperature water bath at 50°C for 2 hours; filter the extract, then concentrate the filtrate into an extract under a vacuum of 0.08 and a temperature of 45°C, and dry the obtained extract to obtain areca nut pigment.

Tests show that under the above conditions, the extraction rate of arecoline can be increased by 15.6% and the extraction rate of pigment can be increased by 39.6% compared with the common solvent extraction method under the above conditions.

Embodiment two

1. Raw material pretreatment process Select mature betel nut fruit, wash, remove the green clothes, remove the betel nut inner germ, then shred, dry at 45°C, crush the dried betel nut, and pass through a 60-mesh sieve to obtain betel nut powder.

2. Extraction preparation process According to the mass/volume ratio, add ammonia water and anhydrous ether to the betel nut powder at a ratio of 1:1 and 1:15 respectively, and then use ultrasonic treatment for 60 minutes (frequency 28kHz, temperature 35°C) ; Filter, collect the filtrate, wash the filter residue with anhydrous ether repeatedly 3 times, combine the ether extracts, and then concentrate under reduced pressure to an extract.

3. Alkaloid extraction process Add 5 times the volume of 0.1mol/L HCl to the above extract, fully dissolve, filter, and collect the filtrate; adjust the pH of the filtrate to 7.0 with ammonia water, and then add it in a ratio of 1:10 (v/v) Chloroform, repeated extraction three times, filtered, combined chloroform extracts; concentrated under reduced pressure, dried to obtain areca nut alkaloids.

4. Pigment extraction process Take the filter residue obtained in step 2, add 50% ethanol solution containing 0.1mol/L HCl at a ratio of 1:30 according to the mass/volume ratio, and ultrasonically treat for 60 minutes (frequency 28kHz, temperature 35°C), and then Extract in a constant temperature water bath at 70°C for 2 hours; filter the extract, then concentrate the filtrate into an extract under a vacuum of 0.08 and a temperature of 45°C, and dry the obtained extract to obtain areca nut pigment.

Tests show that under the above conditions, the extraction rate of arecoline can be increased by 20.1% and the extraction rate of pigment can be increased by 33.8%.

Claims (3)

1. A method for extracting betel nut alkaloids and pigments from betel nuts by an ultrasonic-assisted method, characterized in that: comprising raw material pretreatment process, extract preparation process, alkaloid extraction process, and pigment extraction process, its concrete steps are as follows: 1) The raw material pretreatment process selects mature betel nut fruit, washes, removes green clothes, removes endogerm, then shreds, dries, and pulverizes to obtain betel nut powder; 2) During the preparation of the extract, add ammonia water and anhydrous ether to the betel nut powder at a ratio of 1:1 and 1:10 to 1:15 according to the mass/volume ratio, and then use ultrasonic treatment for 30 to 60 minutes; Filter, collect the filtrate, and concentrate the filtrate to an extract; 3), alkaloid extraction process: add acidic solution to the above extract, filter after fully dissolving, and collect the filtrate; adjust the pH of the filtrate to 7.0 with ammonia water, then add chloroform for extraction to obtain the extract; concentrate under reduced pressure and dry to obtain betel nut Alkaloids; 4) In the pigment extraction process, take the filter residue obtained in step 2, add acidic ethanol solution at a ratio of 1:20 to 1:30 according to the mass/volume ratio, ultrasonically treat for 30 to 60 minutes, and then extract in a constant temperature water bath at 50 to 70°C ; Filtrate the extract, then concentrate the filtrate under reduced pressure until concentrated into an extract, and then dry to obtain the areca nut pigment. 2. The method for simultaneously extracting areca nut alkaloids and pigments from betel nuts by ultrasonic-assisted method according to claim 1, characterized in that: the acidic solution is hydrochloric acid. 3. The method for simultaneously extracting areca nut alkaloids and pigments from betel nuts by ultrasonic-assisted method according to claim 1, characterized in that: the acidic ethanol solution is 50% ethanol with HCl added.