CN101601461A - The extracting method of fresh chive oil - Google Patents

Abstract

The invention provides a kind of extracting method of chive oil, this method may further comprise the steps: (1) gets the fresh chive cut-flower, add its weight 0.02～0.2% (w: emulsifier span w) and 50～200% (w: salad oil v), behind the milled mixture, be 25～55 ℃, microwave power (W) with the ratio of material flow (L/h) in temperature be to carry out continuous microwave under 10～55 the condition to extract, filtrate and filter residue are collected in press filtration; (2) get step (1) gained filtrate, remove the lurid water of sub-cloud, get the green oil phase in upper strata, centrifugally further remove remaining water through separatory, add oil phase 1～10% (v: the dry 10min～3h of calcium chloride w), filter, must clarify dark green chive oil.The inventive method can make fragrance and the taste composition stripping fast at low temperatures in the chive, has not only greatly improved extraction efficiency, and the content of taste composition in the chive oil also has been significantly increased.

Description

The extracting method of fresh chive oil

Technical field

The present invention relates to the Food Chemistry field, is specifically related to the extracting method of the extracting method, particularly scallion oil of fragrance and taste composition in the plant.

Background technology

Green onion (Allium fistulosum) is the perennial herb liliaceous plant, is that compatriots are familiar with and widely used flavouring, especially fresh chive (Allium schoenoprasum L.), and its color and luster is dark green, the pure and fresh fragrance of smell.Contain multiple composition in the chive, as thioether, steroidal, flavones and nitrogen-containing compound etc. to the human body beneficial.But bright green onion water content trial of strength is high, perishable, and local flavor is deterioration very easily, so storage life is very short, and preservation condition is very harsh, is unfavorable for transporting and depositing.Fresh scallion oil has kept the characteristics of chive to greatest extent, and its shelf-life can prolong, so great application prospect is all arranged in flavouring industry and health products trade.

At present, extracting in the fresh spice method of fragrance and taste composition mainly is to adopt steam distillation, distillation-extraction method, solvent extraction and supercritical carbon dioxide extraction method simultaneously.Steam distillation and simultaneously the extraction temperature of distillation-extraction method is higher, the thermal sensitivity composition in the destructible fresh chive is difficult to keep the faint scent and the flavour of chive, and length consuming time, yield are low; The usual vehicle extraction is long required heat time heating time, makes the local flavor slaking of chive, and the fragrance loss that higher vacuum also makes chive in the concentration process totally; The extractant CO that supercritical methanol technology adopts ₂Polarity lower, be unsuitable for the extraction of the more honest and cleaner active ingredients in natural plants of the fresh plant of high-moisture or price.

Granted publication number discloses the extracting method of a scallion oil for the patent of invention of CN 1088342C, this method with edible salad oil be solvent, through the lixiviate of long-time lower temperature, after crude extract separated, filter and dewater promptly get scallion oil.Above-mentioned patent at first needs 3-7 days, 25-55 ℃ extraction, and fragrance ingredient polarity is close in the polarity of selected extractant salad oil and the chive, mainly proposes wherein volatile ingredient.Damp as seen by the pistac of its product, the distinctive aquamarine of chive proposes as yet, and the composition close with green polarity, particularly non-volatile flavour composition proposes as yet.

Summary of the invention

The technical problem to be solved in the present invention is under the prerequisite of careful reservation chive fresh flavor and color and luster feature, the content of fragrance and taste composition in the raising chive oil.

The technical scheme that the present invention addresses the above problem is:

The extracting method of fresh chive oil, this method may further comprise the steps:

(1) gets fresh chive (Allium schoenoprasum L.) cut-flower, 0.02～0.2% the emulsifier span (w: w) and 50～200% (w: salad oil v) that adds its weight, behind the milled mixture, be 25～55 ℃, microwave power (W) with the ratio of material flow (L/h) in temperature be to carry out continuous microwave under 10～55 the condition to extract, filtrate and filter residue are collected in press filtration;

(2) get step (1) gained filtrate, remove the lurid water layer of sub-cloud, get the green oil phase liquid in upper strata through separatory, centrifugal remaining water, adding oil phase volume 1～10% (v: calcium chloride w), dry 10min～3h of further removing, filter, must clarify dark green chive oil.

The chive filter residue last through said extracted is that solvent further extracts with acetone and benzinum mixed liquor, and concrete grammar is as follows: get step (1) gained filter residue, add 1～4 times of its weight (w: acetone benzinum mixed liquor v); Be 25～55 ℃, microwave power (W) with the ratio of material flow (L/h) in temperature then be to carry out continuous microwave under 10～55 the condition to extract; Suction filtration is got filtrate; In gained filtrate with salt to saturated, leave standstill, wait to be divided into and get supernatant liquid after two-layer, 30～50 ℃ of following decompression distillation, must clarify dark green chive oil, last and the merging of step (2) gained chive oil; Used acetone benzinum mixed liquor is by acetone: the volume ratio of benzinum=1: 1～1: 10 is mixed and is obtained.

The inventive method gained chive oil must be preserved down at-17 ℃.

The inventive method is utilized the non-thermal effect of microwave and to the broken wall effect of plant cell, make fragrance and taste composition stripping fast at a lower temperature in the bright green onion, avoid the destruction of thermal sensitivity composition in leaching process in the bright green onion, effectively kept the local flavor of fresh chive; This method is adding food grade emulsifier sapn (w/o type) with salad oil on as the basis of extractant, utilize sapn the role of phase transfer in the profit two-phase, impel bright green onion Semi-polarity widely distributed fragrance and taste composition to enter oil phase, effectively proposed the local flavor and the color and luster feature of chive and improved extraction efficiency; In order further to improve recovery rate, also available high polarity and lower boiling solvent (acetone benzinum mixed liquor) extract remaining chive slag after above-mentioned steps, residual fragrance and taste composition are extracted, to reach the purpose that improves scallion oil concentration and fully carry flavor components in the most green onion.

The present invention finds that by the color of brighter scallion oil and the relation of local flavor the depth of the green of scallion oil can be used as index, and in order to judge the concentration height of the contained flavor components of scallion oil, table 1 explanation adds before and after the emulsifying agent, the look valency of the scallion oil of carrying and the relation between local flavor.The visible color valency is higher, and flavor components proposes the more.

The relation of table 1 chive oil color and local flavor

The bright scallion oil that table 2 explanation is extracted by technology of the present invention is preserved after 30 days the color of chive oil and the relation of local flavor under different temperatures.The visible color valency is higher, and then the fresh flavor of scallion oil is preserved better.So the look valency can be used as a whether objective indicator of deterioration of scallion oil local flavor:

Table 2 is preserved the sense organ of scallion oil after 30 days and the relation of corresponding look valency

The look valency of scallion oil is defined as: be solvent and be blank that with 60-90 ℃ of benzinum tested sample concentration is 1%, 1cm cuvette, the absorbance at maximum absorption band 430nm place.The detection method of scallion oil look valency is as follows: scallion oil to be measured is dissolved in 60-90 ℃ of benzinum as sample, does blank elimination background influence with benzinum, and in 430nm place test samples absorbance, calculate the look valency as follows.

$E_{1\mathrm{cm}430\mathrm{nm}}^{1\%}=\frac{\mathrm{Af}}{m}\×\frac{1}{100}$

In the formula, E---look valency

The absorbance of A---actual measurement sample

The extension rate of f---scallion oil

The quality of m---scallion oil to be measured (g)

Total look valency=E * V

In the formula, V-scallion oil volume (mL)

Description of drawings

Fig. 1 is that the inventive method gained chive oil is preserved the visible light figure after 30 days under different temperatures, wherein

Represent 25 ℃ of samples of preserving down,

Represent 5 ℃ of samples of preserving down,

Represent-7 ℃ of samples of preserving down,

Represent-17 ℃ of samples of preserving down.

The specific embodiment

The used low-temperature microwave extraction element of following examples is seen patent " low-temperature microwave extraction equipment ", the patent No.: ZL 2005200609603.

Example 1

(1) gets the fresh chive cut-flower, add its weight 0.2% (w: Arlacel-80 w) and 100% (w: salad oil v), behind the milled mixture, change the low-temperature microwave extraction element over to, it is 2400W that microwave power is set, temperature is 25～45 ℃ (the instrument temperature upper limit is set to 45 ℃ and gets final product during practical operation, down with), and material flow is 52L/h; Press filtration, it is standby to collect filtrate and filter residue;

(2) get step (1) gained filtrate, standing demix, separatory remove the light yellow water of lower floor, get the green oil phase in upper strata, and 4000r/min is centrifugal, and further remove and anhydrate, adding oil phase 5% (v: the dry 1h of calcium chloride w), filter, must clarify dark green chive oil A; Recording its look valency with spectrophotometer is 18.31, and oil recovery rate is 67.78%;

(3) change step (1) gained filter residue over to the low-temperature microwave extraction element, add its 2 volume acetone benzinum mixed liquor doubly, acetone: benzinum=1: 1 (v: v), be that 2400W, temperature are that 25～45 ℃, material flow are to extract continuously under the condition of 52L/h at microwave power then, suction filtration is got filtrate; Extremely saturated with salt in gained filtrate, standing demix, separatory are got upper strata bottle green oil phase, 45 ℃ of following decompression distillation, get bottle-green chive oil B; Recording its look valency with spectrophotometer is 19.59, oil recovery rate 23.72%;

(4) merge chive oil A and scallion oil B, promptly get chive oil, recording its total look valency with spectrophotometer is 37.90, total oil recovery rate 91.50%.

Example 2

(1) get the fresh chive cut-flower, add the Arlacel-60 of its weight 0.02% and 50% salad oil, behind the milled mixture, change the low-temperature microwave extraction element over to, it is 1600W that microwave power is set, and temperature is 25～35 ℃, and material flow is that 30L/h extracts continuously; Press filtration, it is standby to collect filtrate and filter residue;

(2) get step (1) gained filtrate, standing demix, separatory remove the light yellow water of lower floor, get the green oil phase in upper strata, and 4000r/min is centrifugal, and further remove and anhydrate, adding oil phase 2% (v: the dry 2h of calcium chloride w), filter, must clarify dark green chive oil A; Recording its look valency with spectrophotometer is 14.81, and oil recovery rate is 51.23%;

(3) change step (1) gained filter residue over to the low-temperature microwave extraction element, add doubly (w: acetone benzinum mixed liquor v) of its 4 volume, acetone: benzinum=1: 5 (v: v), then microwave power be 1600W, temperature be 25～35 ℃,, material flow is to extract continuously under the condition of 30L/h, suction filtration is got filtrate; Extremely saturated with salt in gained filtrate, standing demix, separatory are got upper strata bottle green oil phase, 35 ℃ of following decompression distillation, get bottle-green chive oil B; Recording its look valency with spectrophotometer is 21.47, oil recovery rate 23.72%;

(4) merge chive oil A and scallion oil B, promptly get chive oil, recording its total look valency with spectrophotometer is 36.28, total oil recovery rate 91.51%.

Example 3

(1) get the fresh chive cut-flower, add the Arlacel-20 of its weight 0.01% and 200% salad oil and blend together, change the low-temperature microwave extraction element over to, it is 3200W that microwave power is set, and temperature is 25～55 ℃, and material flow is that 200L/h extracts continuously; Press filtration, it is standby to collect filtrate and filter residue;

(2) get step (1) gained filtrate, standing demix, separatory remove the light yellow water of lower floor, get the green oil phase in upper strata, 4000r/min is centrifugal, further removes and anhydrates, adding oil phase 10% (v: the dry 20min of calcium chloride w), filter, must clarify dark green chive oil A; Recording its look valency with spectrophotometer is 19.64, and oil recovery rate is 69.23%;

(3) change step (1) gained filter residue over to the low-temperature microwave extraction element, add and slag equal-volume (w: acetone benzinum mixed liquor v), acetone: benzinum=1: 5 (v: v), then microwave power be 3200W, temperature be 25～50 ℃,, material flow is to extract continuously under the condition of 200L/h, suction filtration is got filtrate; Extremely saturated with salt in gained filtrate, standing demix, separatory are got upper strata bottle green oil phase, 45 ℃ of following decompression distillation, get bottle-green chive oil B; Recording its look valency with spectrophotometer is 15.87, oil recovery rate 28.28%;

(4) merge chive oil A and scallion oil B, promptly get chive oil, recording its total look valency with spectrophotometer is 35.51, total oil recovery rate 92.51%.

Example 4

(1) get the fresh chive cut-flower, add the Arlacel-80 of its weight 0.01% and 150% salad oil and blend together, change the low-temperature microwave extraction element over to, it is 4800W that microwave power is set, and temperature is 25～50 ℃, and material flow is that 400L/h extracts continuously; Press filtration, it is standby to collect filtrate and filter residue;

(2) get step (1) gained filtrate, standing demix, separatory remove the light yellow water of lower floor, get the green oil phase in upper strata, 4000r/min is centrifugal, further removes and anhydrates, adding oil phase 5% (v: the dry 40min of calcium chloride w), filter, must clarify dark green chive oil A; Recording its look valency with spectrophotometer is 20.65, and oil recovery rate is 70.03%;

(3) change step (1) gained filter residue over to the low-temperature microwave extraction element, add and slag equal-volume (w: acetone benzinum mixed liquor v), acetone: benzinum=1: 1.5 (v: v), then microwave power be 4800W, temperature be 25～50 ℃,, material flow is to extract continuously under the condition of 400L/h, suction filtration is got filtrate; Extremely saturated with salt in gained filtrate, standing demix, separatory are got upper strata bottle green oil phase, 45 ℃ of following decompression distillation, get bottle-green chive oil B; Recording its look valency with spectrophotometer is 16.58, oil recovery rate 24.17%;

(4) merge chive oil A and scallion oil B, promptly get chive oil, recording its total look valency with spectrophotometer is 37.03, total oil recovery rate 94.20%.

(in the foregoing description 1～4, each goes on foot the look valency and all calculates with the bright scallion oil that green onion is carried of 30g with total look valency, with the incommensurability of avoiding the quantity of solvent difference to bring.)

Claims (2)

1, the extracting method of chive oil, this method may further comprise the steps:

(1) gets the fresh chive cut-flower, 0.02～0.2% (w: emulsifier span w) and 50～200% (w: salad oil v) that adds its weight, behind the milled mixture, be 25～55 ℃, microwave power (W) with the ratio of material flow (L/h) in temperature be to carry out continuous microwave under 10～55 the condition to extract, filtrate and filter residue are collected in press filtration;

(2) get step (1) gained filtrate, remove the lurid water layer of sub-cloud, get the green oil phase liquid in upper strata through separatory, centrifugal remaining water, adding oil phase volume 1～10% (v: calcium chloride w), dry 10min～3h of further removing, filter, must clarify dark green chive oil.

2, extracting method as claimed in claim 1 is characterized in that further comprising the steps of:

Get step (1) gained filter residue, the acetone benzinum mixed liquor that adds 1～4 times of its weight, acetone: benzinum=1: 1～1: 10 (v: v), be 25～55 ℃, microwave power (W) with the ratio of material flow (L/h) in temperature then be to carry out continuous microwave under 10～55 the condition to extract; Suction filtration is got filtrate; In gained filtrate with salt to saturated, leave standstill, upper oil phase is got in layering, 30～50 ℃ of following decompression distillation, must clarify dark green chive oil, last and step (2) gained chive oil merge chive oil.

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