CN1316494A

CN1316494A - Process for extracting antioxidizing agent and perfume from rosemary

Info

Publication number: CN1316494A
Application number: CN00112834A
Authority: CN
Inventors: 张高; 陈德茂; 巫华美; 康兴屏
Original assignee: Individual
Current assignee: Individual
Priority date: 2000-04-06
Filing date: 2000-04-06
Publication date: 2001-10-10

Abstract

A process for extracting antioxidizing agent and perfume from rosemary includes such steps as pulverizing fresh ro semary plant by cell pulverizing method to obtain cell tissue substance, immersing in inorganic alkali solution, separating solution from dregs, removing impurites from solution to obtain solution A, neutralizing dregs, drying, extracting in organic solvent, concentrating to obtain B, the membrane filtering, concentrating and drying of A to obtain refined antioxidizing agent, supercritical extraction of B, concentrating and drying to obtain antioxidizing agent and perfume. Its advantages are high extraction efficiency and low cost.

Description

Obtain the production method of antioxidant and spices in the Rosmarinus officinalis

The present invention relates to a kind of production method of from rosemary plant, obtaining antioxidant and spices.

The processing technology of the former plant of Rosmarinus officinalis is mainly divided two portions, and the one, the extraction of Rosmarinus officinalis spices, the 2nd, the extraction separation of antioxidant.At present, obtain the antioxidant in the rosemary plant and the method for spices in the prior art and generally adopt inorganic solvent extraction method, organic solvent extraction method and three kinds of main method of supercritical carbon dioxide extraction method, though the inorganic solvent extraction method has the higher and low advantage of tooling cost of relative yield, but exist but that product purity is not enough, band impurity color, be shortcoming such as peculiar smell, thereby its use range is restricted; Though the organic solvent extraction method has the advantage that technology is simple, investment is less, exist that yield is low, the organic solvent residual height of product, the higher shortcoming of tooling cost; Though and supercritical carbon dioxide process has the low advantage of the organic solvent residual of its product, its production unit is once invested too big, general unable the bearing of domestic enterprise.

The objective of the invention is: the production method of obtaining antioxidant and spices in the Rosmarinus officinalis that provides that a kind of extraction yield is higher, product purity is higher, investment is less, production cost is lower.

The present invention is achieved in that its former plant of Rosmarinus officinalis after will cleaning pulverizes with the cell pulverization method under fresh state, get the cell grade tissue substance, inorganic alkali solution with PH8～12 is to extract solvent impregnated this tissue substance, get the lixiviate mixture, with the lixiviate mixture by centrifugal solid-liquid separate solution and residue, solution part is carried out earlier after neutralization precipitation handles, remove wherein most of pectin through separating technology again, Mierocrystalline cellulose, protein impurities, its surplus solution is the crude extract A that contains antioxidant, gets the crude extract B that mainly contains spices and antioxidant and other impurity after in the residue and dry back is concentrated with organic solvent extraction; Crude extract A is carried out membrane filtration, slough wherein remaining bigger pectin, Mierocrystalline cellulose, protein and other polysaccharide impurity of molecular weight, adjusting membrane pore size can remove pigment and smell substance among the crude extract A, the crude extract A behind the membrane filtration is carried out promptly getting after reverse osmosis or spray method concentrate drying are handled make with extra care antioxidant product; With the super critical extraction of adding entrainment agent crude extract B is handled, entrainment agent can adopt ethanol, methyl alcohol, acetone, acetic ester, methylene dichloride, ethane, propane, water, promptly gets antioxidant and Rosmarinus officinalis spice product after adopting reverse osmosis or spray method concentrate drying to handle again; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract A, makes and handle, further to remove variegated, peculiar smell and the impurity in its antioxidant; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract B, makes and handle, or adopt membrane filtering method to handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.

Owing to adopted technique scheme, the present invention adopts the cell pulverization method to make the cell rupture of rosemary plant, various effective ingredients or invalid impurity ooze out, its antioxidant can fully be contacted with the extraction solvent, thereby improved extraction yield greatly, the supercritical methanol technology of Cai Yonging is that plant material is directly handled in the prior art, and the supercritical methanol technology that adopts in the present invention just is used for the processing of crude extract B, therefore its treatment capacity is 1/tens of a direct facture, so the volume of its equipment and also corresponding the significantly reducing of investment, and the present invention adds entrainment agent in supercritical carbon dioxide process, has solved crude extract B at one stroke and has removed peculiar smell, separate spices, obtain the problem of antioxidant; Extract all essential high temperature that adopts of antioxidant in the prior art; and antioxidant oxidation voluntarily easily under hot conditions; in order to obtain high in antioxidants; prior art generally adopts high temperature extraction under the nitrogen protection; thereby increased production cost; and the present invention adopts cytoclasis earlier; increase the solvent contact area; again adopt normal temperature art breading such as membrane sepn supercritical methanol technology, the precipitator method, macroporous resin column chromatography thereafter; effectively compensate the extraction yield loss that high temperature brings, thereby solved extraction yield and this contradiction of oxidation-resistance effectively.Therefore, the present invention compared with prior art has the advantage that extraction yield is higher, product purity is higher, investment is less, production cost is lower.

Embodiments of the invention: the former plant of the Rosmarinus officinalis after will cleaning is crushed to 1～10 order with the cell pulverization method under fresh state, the cell grade tissue substance, be solvent impregnated this tissue substance of extraction with the inorganic alkali solution of PH8～12, mineral alkali can adopt Na ₂CO ₃, NaHCO ₃, NaOH, K ₂CO ₃, KHCO ₃Basic metal such as KOH series weak base formula highly basic or its mixture, steeping process carries out at normal temperatures, tissue substance gets the lixiviate mixture behind dipping, with the lixiviate mixture by centrifugal solid-liquid separate solution and residue, solution part is carried out earlier after neutralization precipitation handles, remove wherein most of pectin through separating technology again, Mierocrystalline cellulose, protein impurities, its surplus solution is the crude extract A that contains antioxidant, after in the residue and dry back concentrated with organic solvent extraction mainly contain the crude extract B of spices and antioxidant and other impurity, crude extract A is carried out membrane filtration, membrane filtration can adopt millipore filtration, the single filtration of ultrafiltration and reverse osmosis or its combination filtration procedure, slough the bigger pectin of molecular weight remaining among the crude extract A, Mierocrystalline cellulose, protein and other polysaccharide impurity, adjusting membrane pore size can remove pigment and smell substance among the crude extract A, the crude extract A behind the membrane filtration is carried out promptly getting after reverse osmosis or spray method concentrate drying are handled make with extra care antioxidant product; With the super critical extraction of adding entrainment agent crude extract B is handled, entrainment agent can adopt ethanol, methyl alcohol, acetone, acetic ester, methylene dichloride, ethane, propane, water, during processing, the operating pressure of its extractor is controlled at 100atm～200atm, its working temperature is controlled between 20 ℃～40 ℃, promptly gets antioxidant and Rosmarinus officinalis spice product after adopting reverse osmosis or spray method concentrate drying to handle again; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract A, makes and handle, further to remove variegated, peculiar smell and the impurity in its antioxidant; Also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract B, makes and handle, or adopt membrane filtering method to handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.When adopting the macroporous adsorbent resin method to carry out the column chromatography processing, its column temperature preferably maintains between 20 ℃～40 ℃, and its organic solvent can adopt methyl alcohol, ethanol, acetone and the aqueous solution thereof or its mixture.

Claims

1, a kind of production method of obtaining antioxidant and spices in the Rosmarinus officinalis, it is characterized in that: the Rosmarinus officinalis after will cleaning is pulverized with the cell pulverization method under fresh state by former plant, get the cell grade tissue substance, inorganic alkali solution with PH8～12 is to extract solvent impregnated this tissue substance, get the lixiviate mixture, with the lixiviate mixture by centrifugal solid-liquid separate solution and residue, solution part is carried out earlier after neutralization precipitation handles, remove wherein most of pectin through separating technology again, Mierocrystalline cellulose, protein impurities, its surplus solution is the crude extract A that contains antioxidant, gets the crude extract B that mainly contains spices and antioxidant and other impurity after in the residue and dry back is concentrated with organic solvent extraction; Crude extract A is carried out membrane filtration, slough wherein remaining bigger pectin, Mierocrystalline cellulose, protein and other polysaccharide impurity of molecular weight, adjusting membrane pore size can remove pigment and smell substance among the crude extract A, the crude extract A behind the membrane filtration is carried out promptly getting after reverse osmosis or spray method concentrate drying are handled make with extra care antioxidant product; With the super critical extraction of adding entrainment agent crude extract B is handled, entrainment agent can adopt ethanol, methyl alcohol, acetone, acetic ester, methylene dichloride, ethane, propane, water, promptly gets antioxidant and Rosmarinus officinalis spice product after adopting reverse osmosis or spray method concentrate drying to handle again.

2, the production method of obtaining antioxidant and spices in the Rosmarinus officinalis according to claim 1, it is characterized in that: also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract A, makes and handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.

3, the production method of obtaining antioxidant and spices in the Rosmarinus officinalis according to claim 1, it is characterized in that: also can under normal temperature condition, adopt the macroporous adsorbent resin method to carry out column chromatography for the antioxidant product that from crude extract B, makes and handle, or adopt membrane filtering method to handle, further to remove variegated, peculiar smell and the impurity in its antioxidant.