CN104928012A - Method for extracting tea oil by demulsification based on aqueous enzymatic method - Google Patents

Abstract

The invention discloses a method for extracting tea oil by demulsification based on an aqueous enzymatic method. The method comprises the following steps: processing tea seed powder by microwaves for 60 to 120 seconds; adding distilled water at a material-liquid mass ratio of 1:4 to 1:8, pulping, and collecting upper-layer emulsified liquid; pulping the residual water phase and residues again, and collecting upper-layer emulsified liquid; combining the collected emulsified liquid; adding 0.5-6% of composite enzymatic hydrolysis liquid based on the total mass of the emulsified liquid, performing water bath enzymolysis, centrifuging, and taking upper-layer tea oil; adding an ethanol solution into the residual emulsified liquid, performing water bath treatment, centrifuging, and collecting upper-layer tea oil; combining the collected tea oil, an drying in vacuum. According to the method, the emulsified liquid is high in oil content, and the process is simple, novel and practical; the emulsified liquid is subjected to composite enzyme hydrolysis and ethanol demulsification, so that the enzymatic hydrolysis volume is greatly reduced, the enzyme consumption is greatly reduced, and the process is economic and efficient; microwaves, enzymatic hydrolysis and ethanol are adopted for assisting in oil extraction, so that natural active ingredients of the tea oil are better preserved, and the oil extraction process is safe and nutritive.

Description

A kind of method extracting tea oil based on aqueous enzymatic method breakdown of emulsion

Technical field

The invention belongs to grain and oil manufacture field.Relate to the extracting method of tea oil.

Background technology

The extractive technique of tea-seed oil mainly contains conventional press method, organic solvent lixiviation process, soxhlet extraction methods, supercritical extraction, water substitution and aqueous enzymatic method etc.Industrial conventional milling process and organic solvent lixiviation process.

Milling process Residual oil is higher, and its grouts residual oil content is up to 8 ~ 12%, and pyroprocessing makes its nutritive ingredient destroy, as cake protein matter serious degenerative, and during squeezing the tea seed episperm that mixes to make grouts contain xylogen very high, be difficult to utilize; Solvent extraction method exists that facility investment is large, product exists the safety issues such as dissolvent residual; The problems such as it is high that supercritical extraction exists equipment investment, and production cost is high, and color and luster is poor; Water law (water substitution and aqueous enzymatic method general name) is the oil extracting methods of a kind of alternative organic molten Ji " safety, efficient, economy ", and the tea oil quality raised is high, and activeconstituents retention is good.But water law is put forward the serious emulsification phenomenon produced in oily process and caused its oil extracting rate extremely low, it is restriction camellia seed oil water-swollen squid " bottleneck " problem, and need during aqueous enzymatic method breakdown of emulsion to use enzyme amount too large, cost is too high, and therefore, water law oil extracting process needs to study improvement further.

Summary of the invention

The object of the invention is to propose a kind of safe, simple, efficient, economic Oleum Camelliae extraction novel method.

Concrete technology step of the present invention is as follows.

(1) tea seed manually shells, and dry, pulverize.

(2) a certain amount of tea seed powder is taken, microwave 60-120 s.

(3) add distilled water with feed liquid mass ratio 1:4 ~ 1:8, colloidal mill making beating 10-15 min, in the centrifugal 10-30 min of 3000-10000 r/min, collects upper strata emulsion.

(4) by remaining aqueous phase and residue colloidal mill making beating 5-10 min again, leave standstill, in the centrifugal 10-30 min of 3000-10000 r/min, collect upper strata emulsion.

(5) emulsion collected of combining step (3) and (4).

(6) in emulsion, add the complex enzyme hydrolysis liquid that emulsion total mass is 0.5-6 %, after 40-60 DEG C of water enzyme digestion 2-6 h, in the centrifugal 5-10 min of 3000-10000 r/min, get upper strata edible vegetable oil; Prozyme is proteolytic enzyme, phosphide enzyme, polygalacturonase and amylase, and content is respectively 0.2-2%, 0.2-2%, 0-2% and 0-2%.

(7) in remaining emulsion, add solid-to-liquid ratio be again the concentration of 1:1-6 is 40-60% ethanolic soln, and 2-6 h is extracted in water-bath, collected by centrifugation upper strata edible vegetable oil.

(8) edible vegetable oil collected of combining step (6) and (7), vacuum-drying.

Principal feature of the present invention is.

1, utilize microwave and colloidal mill making beating fully to destroy oil body cell, promote the abundant formation of emulsion, the emulsification degree of oil is very high, therefore, just can be reached the effect of isolate oil body by simple centrifuging process.

2, go out the high emulsion of oil length by centrifugation, then carry out complex enzyme zymohydrolysis and ethanol two step breakdown of emulsion to emulsion, breakdown of emulsion is complete, and emulsion small volume, greatly reduces by enzyme amount, and technique is simple, economical.

3, adopt microwave, enzymolysis and ethanol assisted Extraction oil, the active skull cap components of tea oil is preserved better, the lurid color and luster of tea oil is kept, oil extracting process safe nutrition.What the present invention adopted is that aqueous enzymatic method extracts tea oil from camellia seed kernel, first form emulsion, then breakdown of emulsion carries oil, few by enzyme amount, does not use organic reagent, greatly reduces cost.

Embodiment

Below in conjunction with embodiment, the present invention is described in further detail, but the non-scope being only limitted to these embodiments of scope of the present invention should be understood.

Embodiment 1.

1, tea seed manually shells, and dry, pulverize.

2, take 50 g tea seed powder, microwave 100 s, adding distil water extracts, and solid-liquid ratio is 1:5, and colloidal mill is pulled an oar 13 min, and 4200 r/min are centrifugal, centrifugal 21 min, repeat 3 times, collection emulsion.

3, by remaining aqueous phase and residue again colloidal mill to pull an oar 9 min, leave standstill, centrifugal 15 min of 4200 r/min, repeat 3 times, collection emulsion.

4, the emulsion of twice collection is merged.

5, in the emulsion merged, add proteolytic enzyme, 1.5% phosphide enzyme and 0.5% amylase that massfraction is 1%, at 50 DEG C, enzymolysis 3 h, centrifugal, gets upper strata edible vegetable oil.

6, in remaining emulsion, add solid-to-liquid ratio be again the concentration of 1:1 is 40% ethanolic soln, and 4 h are extracted in water-bath, collected by centrifugation upper strata edible vegetable oil.

7, merge edible vegetable oil, vacuum-drying, oil extracting rate is 85.78%.

Embodiment 2.

1, tea seed manually shells, and dry, pulverize.

2, take 1 kg tea seed powder, microwave 80 s, adding distil water extracts, and solid-liquid ratio is 1:4, and colloidal mill is pulled an oar 12 min, and 5000 r/min are centrifugal, centrifugal 23 min, repeat 3 times, collection emulsion.

3, by remaining aqueous phase and ultrasonic 20 min of residue, colloidal mill is pulled an oar 10 min again, and leave standstill, 4200 r/min are centrifugal, centrifugal 12 min, repeat 3 times, collection emulsion.

4, the emulsion of twice collection is merged.

5, add in the emulsion merged massfraction be 1% proteolytic enzyme, 1% phosphide enzyme, 0.5% polygalacturonase and 0.5% amylase, in 45 DEG C of enzymolysis 2.5 h, centrifugal, get upper strata edible vegetable oil.

6, in remaining emulsion, add solid-to-liquid ratio be again the concentration of 1:6 is 45% ethanolic soln, and 4 h are extracted in water-bath, collected by centrifugation upper strata edible vegetable oil.

7, merge edible vegetable oil, vacuum-drying, oil extracting rate is 82.65%.

Embodiment 3.

1, tea seed manually shells, and dry, pulverize.

2, take 60 g tea seed powder, microwave 70 s, adding distil water extracts, and solid-liquid ratio is 1:7, and colloidal mill is pulled an oar 15 min, and 4500 r/min are centrifugal, centrifugal 25 min, repeat 3 times, collection emulsion.

3, by remaining aqueous phase and residue microwave 90 s, colloidal mill is pulled an oar 8 min again, and leave standstill, 4200 r/min are centrifugal, centrifugal 13 min, repeat 3 times, collection emulsion.

4, the emulsion of twice collection is merged.

5, in the emulsion merged, proteolytic enzyme, 1% phosphide enzyme and 0.5% polygalacturonase that massfraction is 1% is added, in 60 DEG C of enzymolysis 6 h, centrifugal, get upper strata edible vegetable oil.

6, in remaining emulsion, add solid-to-liquid ratio be again the concentration of 1:3 is 50% ethanolic soln, and 4 h are extracted in water-bath, collected by centrifugation upper strata edible vegetable oil.

7, merge edible vegetable oil, vacuum-drying, oil extracting rate is 87.29%.

Claims (1)

1. extract a method for tea oil based on aqueous enzymatic method breakdown of emulsion, it is characterized in that step is as follows:

(1) tea seed manually shells, and dry, pulverize;

(2) a certain amount of tea seed powder is taken, microwave 60-120 s;

(3) add distilled water with feed liquid mass ratio 1:4 ~ 1:8, colloidal mill making beating 10-15 min, in the centrifugal 10-30 min of 3000-10000 r/min, collects upper strata emulsion;

(4) by remaining aqueous phase and residue colloidal mill making beating 5-10 min again, leave standstill, in the centrifugal 10-30 min of 3000-10000 r/min, collect upper strata emulsion;

(5) emulsion collected of combining step (3) and (4);

(6) in emulsion, add the complex enzyme hydrolysis liquid that emulsion total mass is 0.5-6 %, after 40-60 DEG C of water enzyme digestion 2-6 h, in the centrifugal 5-10 min of 3000-10000 r/min, get upper strata edible vegetable oil; Prozyme is proteolytic enzyme, phosphide enzyme, polygalacturonase and amylase, and content is respectively 0.2-2%, 0.2-2%, 0-2% and 0-2%;

(7) in remaining emulsion, add solid-to-liquid ratio be again the concentration of 1:1-6 is 40-60% ethanolic soln, and 2-6 h is extracted in water-bath, collected by centrifugation upper strata edible vegetable oil;

(8) edible vegetable oil collected of combining step (6) and (7), vacuum-drying.