CN103571627A - Preparation method for efficiently extracting allicin - Google Patents

Abstract

The invention relates to the field of allicin and in particular relates to a preparation method for efficiently extracting allicin. The preparation method is characterized in that a process for extracting garlic oil by petroleum ether comprises the following steps: pounding garlic bulbs through a temperature-control multi-purpose high-speed plant tissue pounding machine for a lab (started once per 1 minute under fixed power) for 10 minutes; preprocessing, namely adding exogenous materials, namely 0.175mmol/g of garlic manganese chloride and 0.14mmol/g of garlic glucose in combination with test results of previous parts; coarsely filtering; centrifuging; carrying out organic reagent extraction; centrifuging again; removing residual water; carrying out rotary evaporation to remove all petroleum ether; removing a small amount of residual impurities; blowing nitrogen to remove all petroleum ether so as to obtain the garlic oil. According to the technical scheme, a garlic oil extraction technology is changed, so that the oil yield is increased to be more than 0.25% from 0.17%, the quality guarantee period is prolonged to 1 year from routinely 5 months without any preservative, and the requirements of remote and cross-regional sales are met.

Description

A kind of preparation method of garlicin high efficiency extraction

Technical field

The present invention relates to garlicin field, is a kind of preparation method of garlicin high efficiency extraction.

Background technology

Garlic is Liliaceae per nnial herb, all has cultivation all over the world.According to statistics, the cultivated area of whole world garlic approximately has 113.9 ten thousand hm at present ², more than 1,400 ten thousand tons of Bulbus Allii head annual production.The many provinces of China are all applicable to plantation garlic, and cultivated area reaches 600,000 hm ²1/2 left and right of the total cultivated area of ，Zhan world garlic, 1,000 ten thousand tons of left and right of annual production, account for 75% left and right of Gross World Product, occupy first place in the world.

Garlic and flavour substances thereof are seasonings important in people's daily life, also have very important nourishing function product simultaneously.Yet, since this industry of garlic is medium-term and long-term, also there is following problem: 1, fresh garlic resting stage shorter, in the process of storage, easily go rotten, germinate and rotten, storage tolerance not, after receiving, rate of loss, about 30% left and right, causes very large financial loss to peasant, causes huge waste.2, along with the raising of people's living standard, market is more and more to the needs of garlic product innovation, and exploitation, the working ability of the garlic product innovation of China's adaptation modern market demand are weaker, lack especially the fundamental research to the theory of garlic intensive processing and technology.3, for a long time, its commercialization leading product are unprocessed raw material substantially, and processing variety seldom, and mostly is simple and easy processing, aspect outlet, and main or primary products, added value of product is lower.

In recent years, garlic deep processed product sells well, and the garlic product deep processing in the U.S., Europe has become industry, and it is main evaluation index that the quality of garlic deep processed product quality mainly be take the content of garlicin and Diallyl Thiosulfonate in product.The garlic product of the high allicin content of Devoting Major Efforts To Developing is the trend of garlic deep processing, this can not only fundamentally solve the problem of storage sales difficulty, can also significantly improve economic benefit, adjustment to the Chinese structure of agricultural production, promotes agricultural industrialization process and the generation far-reaching influence of revitalizing the rural economy.Garlic, as the natural agricultural-food of medicine-food two-purpose well received in people's daily life, has unique health care and medicinal function, and garlic goods have a extensive future, and the market requirement increases day by day.

Traditional converted products of current domestic garlic mainly contains quick-frozen garlic goods, comprises pickled product (as pickled garlic rice, sweet and sour garlic); Dehydrated garlic goods: garlic sheet, garlic powder and garlic grain; Fresh-keeping garlic goods are as fresh-keeping garlic rice etc.In China, the pickled product of garlic in the highest flight.The garlic deep processed product of high added value is at the early-stage.The added value of deep processed product is higher, and garlic has special fragrance and fragrance, is also the important source material that is processed into other high value added products.The deep processed product of garlic mainly contains: such as Oleum Bulbus Allii microcapsule, garlicin sheet etc., generally appears in Oleum Bulbus Allii, allicin and garlic polysaccharide with product forms such as capsule, tablets.

At present, the extracting method of Oleum Bulbus Allii is mainly contained to steam distillation, organic solvent lixiviation process, while distillation extraction method, supercritical CO both at home and abroad ₂extraction process etc.:

1, steam distillation: it is the traditional method that current domestic Oleum Bulbus Allii extracts, cardinal principle is the immiscible system that garlic and water form profit, during heating, along with increasing of temperature, essential oil and water all will be accelerated evaporation, produce mixture steam, its steam imports the liquid mixture that obtains water and essential oil in condenser, after oily water separation, can obtain Bulbus Allii quintessence oil product.Principal feature is easy to operate, and equipment is simple, and cost is lower, but Oleum Bulbus Allii yield is lower, the local flavor of products obtained therefrom, far away not as good as the local flavor of fresh garlic, is mainly because active substance is as low in the content of allicin in gained Oleum Bulbus Allii, mostly is micromolecular sulfocompound.

2, organic solvent lixiviation process: lixiviation process extraction oil is similar this principle that mixes, utilizes Oleum Bulbus Allii to be soluble in normal hexane, sherwood oil, ether, this character of ethanol equal solvent, with solvent by Oleum Bulbus Allii lixiviate out.The advantage of this method is that the temperature in operating process is all not high, little on the impact of the garlic organic sulfide of thermo-sensitivity, therefore it is higher to obtain in Oleum Bulbus Allii allicin content, the stability of allicin is also better, but easily has dissolvent residual.

3, while distillation extraction: simultaneous distillation method (SDE, Simultaneous distillation extraction) be the extracting method of a kind of volatile component of getting up of development in recent years, this method obtains solvent extraction two steps by steam distillation and overhead product and unites two into one.This test is carried out in relatively airtight container, by water vapour phase and organic solvent mutually repeatedly, large-area contact, the extraction of disposable realization to essential oil.The method extraction efficiency is high, and solvent load is few, and extraction gained volatile component does not need subsequent disposal substantially, has simplified operation steps, has saved extraction time, is wet distillation to be extracted to the larger improvement of Oleum Bulbus Allii.

4, supercritical CO ₂extraction process: supercritical fluid extraction (SFE, Super Fluid Extraction) is nearly new and high technology growing up for 20 years, utilizes the special property that fluid has at Near The Critical Point and a series of utilisation technologies that form.The existing stronger gas property to high-viscosity material infiltration of supercutical fluid, has again the solubility property of liquid.This method can obtain pure, high-quality Oleum Bulbus Allii, but production cost is high, equipment is complicated, is also difficult at present large-scale industrial production.

Summary of the invention

The object of the invention is to provide a kind of preparation method of new garlicin high efficiency extraction.

Technical scheme of the present invention is: the technical process that it is characterized in that sherwood oil lixiviate Oleum Bulbus Allii is:

Bulbus Allii head is after stamp mill is smashed to pieces, centrifugal after pre-treatment coarse filtration, carries out organic reagent extraction, then centrifugal treating, removes residuary water, and rotary evaporation, except residual impurity, after nitrogen blowing, is obtained Oleum Bulbus Allii;

Smash to pieces: with use for laboratory temperature control multi-purpose high speed plant tissue stamp mill, smash 10min (constant power, interval 1min starts shooting once) to pieces; Pre-treatment: in conjunction with the test-results of fore portion, allogenic material addition is the Manganous chloride tetrahydrate of 0.175mmol/g garlic, the glucose of 0.14mmol/g garlic; Solid-liquid ratio 1: 7, pH value is 6.5; Ultrasonic Conditions is ultrasonic power 48W, 35 ℃ of ultrasonic temperature, ultrasonic time 32min; Coarse filtration, centrifugal: with centrifugal after two-layer filter cloth coarse filtration, centrifugal condition is 10000g, 15min, room temperature; Sherwood oil lixiviate: adopt sherwood oil (60-90) extraction Oleum Bulbus Allii, sherwood oil addition is 200mL sherwood oil/100g garlic, extracts 2 times, extracts 30min under room temperature; Centrifugal: centrifugal condition is 10000g, 15min; After centrifugal, be divided into successively from top to bottom four layers: sherwood oil-oil reservoir, a small amount of protein layer, the faint yellow aqueous solution, precipitation on a small quantity; Remove residuary water: add anhydrous Na ₂sO ₄to occurring without lenticular thing, pour out immediately supernatant liquid after being placed on the refrigerator overnight of-18 ℃; Revolve evaporation: rotary evaporation eliminates sherwood oil; Remove a small amount of impurity: further nitrogen blowing eliminates sherwood oil and can obtain Oleum Bulbus Allii product.

Owing to having adopted technique scheme, change Oleum Bulbus Allii extractive technique, oil yield is brought up to more than 2.5 ‰ by 1.7 ‰, in the situation that not adding any sanitas, make the quality guaranteed period by 5 months of routine, extend to 1 year, meet the needs of remote and trans-regional sale.

Embodiment

Below in conjunction with embodiment, the present invention is further illustrated.

The technical process of sherwood oil lixiviate Oleum Bulbus Allii is:

Bulbus Allii head is after stamp mill is smashed to pieces, centrifugal after pre-treatment coarse filtration, carries out organic reagent extraction, then centrifugal treating, removes residuary water, and rotary evaporation, except residual impurity, after nitrogen blowing, is obtained Oleum Bulbus Allii;

Smash to pieces: with use for laboratory temperature control multi-purpose high speed plant tissue stamp mill, smash 10min (constant power, interval 1min starts shooting once) to pieces; Pre-treatment: in conjunction with the test-results of fore portion, allogenic material addition is the Manganous chloride tetrahydrate of 0.175mmol/g garlic, the glucose of 0.14mmol/g garlic; Solid-liquid ratio 1: 7, pH value is 6.5; Ultrasonic Conditions is ultrasonic power 48W, 35 ℃ of ultrasonic temperature, ultrasonic time 32min; Coarse filtration, centrifugal: with centrifugal after two-layer filter cloth coarse filtration, centrifugal condition is 10000g, 15min, room temperature; Sherwood oil lixiviate: adopt sherwood oil (60-90) extraction Oleum Bulbus Allii, sherwood oil addition is 200mL sherwood oil/100g garlic, extracts 2 times, extracts 30min under room temperature; Centrifugal: centrifugal condition is 10000g, 15min; After centrifugal, be divided into successively from top to bottom four layers: sherwood oil-oil reservoir, a small amount of protein layer, the faint yellow aqueous solution, precipitation on a small quantity; Remove residuary water: add anhydrous Na ₂sO ₄to occurring without lenticular thing, pour out immediately supernatant liquid after being placed on the refrigerator overnight of-18 ℃; Revolve evaporation: rotary evaporation eliminates sherwood oil; Remove a small amount of impurity: further nitrogen blowing eliminates sherwood oil and can obtain Oleum Bulbus Allii product.

1, carried out garlicin extracting method experimental study, filter out extraction (Petroleum ether extraction agent) and obtain the detected organic compounds containing sulfur of Oleum Bulbus Allii distillation extraction fado simultaneously, especially high with the content yield of Diallytrisin and diallyl disulphide.

2, obtain the technological method that improves garlicin yield, added the extraction of different metal ions and the favourable garlicin of polyol, on this basis, set up the mathematical model of ultrasonic-assisted extraction allicin: Y=2.88-0.079X ₁+ 0.029X ₂+ 0.0295X ₃+ 0.024X ₁x ₂-0.002X ₁x ₃-0.007X ₂x ₃-0.145X ₁ ²-0.134X ₂ ²-0.068X ₃ ², by this model and consider practical situation, the optimal processing parameter obtaining is: ultrasonic power 48W, 35 ℃ of ultrasonic temperature, ultrasonic time 32min.Under above-mentioned top condition, allicin yield is 2.89mg/g, and relatively blank group has been improved 44.9%.

3, utilize modern analysis equipment, adopt GC/MS to carry out Oleum Bulbus Allii composition analysis, compared Different Extraction Method Oleum Bulbus Allii component difference, for theoretical basis has been established in its quality control.

Claims (1)

1. the preparation method of a garlicin high efficiency extraction, the technical process that it is characterized in that sherwood oil lixiviate Oleum Bulbus Allii is: Bulbus Allii head is after stamp mill is smashed to pieces, centrifugal after pre-treatment coarse filtration, carry out organic reagent extraction, then centrifugal treating, remove residuary water, rotary evaporation, except residual impurity, after nitrogen blowing, obtain Oleum Bulbus Allii;

Smash to pieces: with use for laboratory temperature control multi-purpose high speed plant tissue stamp mill, smash 10min (constant power, interval 1min starts shooting once) to pieces; Pre-treatment: in conjunction with the test-results of fore portion, allogenic material addition is the Manganous chloride tetrahydrate of 0.175mmol/g garlic, the glucose of 0.14mmol/g garlic; Solid-liquid ratio 1: 7, pH value is 6.5; Ultrasonic Conditions is ultrasonic power 48W, 35 ℃ of ultrasonic temperature, ultrasonic time 32min; Coarse filtration, centrifugal: with centrifugal after two-layer filter cloth coarse filtration, centrifugal condition is 10000g, 15min, room temperature; Sherwood oil lixiviate: adopt sherwood oil (60-90) extraction Oleum Bulbus Allii, sherwood oil addition is 200mL sherwood oil/100g garlic, extracts 2 times, extracts 30min under room temperature; Centrifugal: centrifugal condition is 10000g, 15min; After centrifugal, be divided into successively from top to bottom four layers: sherwood oil-oil reservoir, a small amount of protein layer, the faint yellow aqueous solution, precipitation on a small quantity; Remove residuary water: add anhydrous Na ₂sO ₄to occurring without lenticular thing, pour out immediately supernatant liquid after being placed on the refrigerator overnight of-18 ℃; Revolve evaporation: rotary evaporation eliminates sherwood oil; Remove a small amount of impurity: further nitrogen blowing eliminates sherwood oil and can obtain Oleum Bulbus Allii product.