CN1288731A

CN1288731A - Slow-releasing concentrated fish oil tablet and its preparation

Info

Publication number: CN1288731A
Application number: CN 00109892
Authority: CN
Inventors: 陈受斯; 刘玉; 刘明彦; 欧阳中林
Original assignee: Individual
Current assignee: Individual
Priority date: 2000-07-12
Filing date: 2000-07-12
Publication date: 2001-03-28
Anticipated expiration: 2020-07-12
Also published as: CN1113657C

Abstract

The composition of high-concentration fish oil slow-release tablet comprises (wt%) fish oil 50, clathrate beta-CD cyclodextrin powder 2-10, slow-reslease tablet ethyl cellulose 5-10, excipient starch 5-10, antioxidant nordihydroguaiaretic acid 0.05-0.1 and corrective 0.1-0.2. Its preparation method includes the following steps: firstly, using CO2 supercrifical extraction and rectification method to prepare fish oil with high concentration and high ratio of DHA/EPA, mixing said fish oil with said other ingredients, uniformly stirring them to make effective component fish oil undergo the processes of clathration, solidification, stabilizing and dispersion treatment, seiving with 0.9 mm seive, drying at 60 deg.C, adding 5-10 portions of talcurm powder and granulating, seiving with 3.6 mm seive, drying at 60 deg.C for 1 hr., and tabletting so as to obtain the invented tablet preparation or pill preparation, and the weight of every tablet is 0.5-1g.

Description

Slow-releasing concentrated fish oil tablet and method for making thereof

The invention belongs to a kind of functional health care product that obtains from natural active matter and preparation method thereof, be specifically related to a kind of slow-releasing concentrated fish oil tablet and method for making thereof.

Domestic and international commercially available fish oil soft capsule, effective ingredient DHA and EPA be liquid, content is low, the ratio of DHA/EPA is little, this product is difficult for preserving, having a fish like smell, enter the human intestines and stomach after, dissolve rapidly, concentration is concentrated, and is difficult for the absorption metabolism.In addition, solvent method, molecularly distilled and general CO ₂Supercritical extraction is difficult to obtain the DHA/EPA of high concentration, high yield, high ratio.

The objective of the invention is to develop a kind of easy preservation, no fishy smell, the high dense slow release fish oil sheet and the method for making thereof of effective ingredient energy slow release.

Dense slow releasing tablet component of height of the present invention and weight ratio thereof are as follows: fish oil 50, clathrate β-CO ring aleurone 2-10, slow releasing agent ethyl cellulose 5-10, excipient starch 5-10, nor-pair of hydrogen guaiaretic acid of antioxidant 0.05-0.1, correctives 0.1-0.2.

Described fish oil is rich in DHA and EPA, adopts the method preparation of narration down, and other various components are all the commercially available prod.

The preparation method of product of the present invention is as follows:

In having the general agitator of seal closure, mix effective ingredient fish oil generation enclose, curing, stable, dispersion by said components and weight ratio; With the screening of the mesh screen of 0.9mm, 60 ℃ are dry down, augment the pelletize of 5-10 part Pulvis Talci, divide granular mixture with the 3.6mm mesh screen, under 60 ℃ dry 1 hour again, powder be pressed into 0.5-1.0 restrain/tablet or pill.

The method for making of described DHA of being rich in and EPA fish oil is a kind of supercritical CO ₂Method of extraction.

Described supercritical CO ₂The temperature of extraction cells is 34-38 ℃, and pressure can change between 11-14MPa, and extractor is a slack tank, is extracted raw material and puts in advance, can carry out intermittence or continued operation.

Described rectification separative element is divided into four sections, and 1 section temperature is 37-39 ℃, and 2 sections is 42-44 ℃, and 3 sections is 47-49 ℃, and 4 sections is 52-54 ℃, and the pressure of whole rectifying column changes between 11-14MPa.

Described rectifying column is a rustless steel replenishing essence fractional distillation column.

The temperature of described separative element is 40-45 ℃, and pressure is 6-6.5MPa, extracts preceding 4 hours, and when rectifying column pressure was 11MPa, isolated refine fish oil was rich in EPA, EPA＞43% wherein, DHA＜28%; Back 4 hours when rectifying column pressure is 15MPa, obtains being rich in the refine fish oil of DHA; DHA＞64% wherein, EPA＜10%, the total recovery of EPA+DHA is up to 90%.

Described supercritical CO ₂Separator, the cyclone separator that similar is general, the extraction mixture behind the cooling decompression tangentially enters described separator, separates back CO ₂Discharge from its top, extract fish oil is discharged from its bottom.

Further detailed explanation of the present invention reaches embodiment in conjunction with the accompanying drawings and is described as follows:

Fig. 1 is two liter extracting rectifying segregation apparatus flow charts.

As shown in the figure, 1 is CO ₂Pump, 2 is the raw material dosing pump, and 3 for giving hot device, and 4 is extraction kettle, and 5 is four sections rectifying columns, and 6 is the separator I, and 7 is the separator II, and 8 is CO ₂Depurator, 9 is condenser, 10 is CO ₂Gas cylinder.

As shown in Figure 1, the rough fish oil ethyl ester raw material of raw material adds extraction kettles 4 through measuring pump 2, reach specified temperature and pressure after, open CO₂Pump 1, CO₂From CO₂Tank 10, condenser 9 through pump 1, give hot device 3 and enter from extraction kettle 4 bottoms, after reaching rated pressure and temperature, enter from the bottom of four sections rectifying columns 5, each section column temperature and post are compressed into capable rectifying from bottom to top, the product that comes out from rectifying column 5 tops, enter separator 6, in case of necessity again through separator 7, CO₂Discharge warp from the separator top Clarifier 8 retrieval systems recycle. The rectifying products obtained therefrom is emitted from the bottom of separator 6 or 7.

Advantage of the present invention is as follows:

1. owing to the DHA of product of the present invention and the content height of EPA, its ratio is protected near function again Strong the best is taken in ratio, so can obtain higher health-care effect.

2. because can slowly-releasing its active ingredient DHA and EPA behind the product introduction human body stomach of the present invention, Be beneficial to and keep its optimum absorption and metabolism.

3. the used fat-soluble high fish oil that is rich in DHA and EPA is through inclusion, curing, one-tenth Powder, and then reached again dispersion, flavoring after the deodorizing, has reduced volatility, has improved stability And non-oxidizability.

4. make tablet, be easy to preserve, taking convenience, good mouthfeel reduces frequency.

The embodiment of the invention is as follows:

Embodiment 1

Adopt flow process shown in Figure 1.Get rough fish oil 400 grams, EPA+DHA＜30% by step recited above, injects extraction kettle 4 with pump 2, injects CO with pump 1 ₂, at 34 ℃ of temperature, pressure 11.0MPa, CO ₂Extract under the flow 14Kg/H, enter four sections rectifying columns then, from bottom to top, 37 ℃ of 1 section column temperatures, 42 ℃ of 2 sections column temperatures, 47 ℃ of 3 sections column temperatures, 52 ℃ of 4 sections column temperatures carry out rectification under the rectifying column 5 outlet pressure 12MPa, after the decompression cooling, the pressure of separator 6 is transferred to 6MPa, when temperature transfers to 40 ℃, with this understanding, 4 hours inner separator 6 bottoms obtain being rich in the fish oil of EPA, wherein, EPA＞43%, DHA＜28%, behind the extracting rectifying 4 hours, post is pressed and is carried to 14.0MPa, obtains being rich in the fish oil of DHA from separator 7 bottoms, wherein DHA＞64%, EPA＜10%, be rich in EPA product 250 grams, be rich in DHA fish oil product 90 grams, total recovery is up to 85%.

Get fish oil 50 grams of above-mentioned DHA of being rich in or EPA, clathrate β-CO cyclodextrin 2 grams, slow releasing agent ethyl cellulose 5 grams, excipient starch 5 grams, the lucky first dioxygen of antioxidant guaiaretic acid 0.05 gram and correctives 0.1 gram, through 60 ℃ of dryings, benefit increases Pulvis Talci 10 grams again, makes powder, crosses the screen cloth of 3.6mm, at 60 ℃ of dryings compression molding after 1 hour, tablet amounts is 0.5 gram/sheet again.

Embodiment 2

Adopt the described flow process of Fig. 1.Rough fish oil ethyl ester 400 grams, EPA+DHA＜30%, 38 ℃ of extraction temperature, pressure 14.0MPa, CO ₂Flow 18Kg/H, 1 section 39 ℃ of rectifying column column temperatures, 2 sections 44 ℃, 3 sections 49 ℃, 4 sections 54 ℃, column outlet pressure 17.0MPa, decompression is cooled to 6.5MPa, 40 ℃, must be rich in EPA fish oil product, wherein EPA＞43% in preceding 4 hours, DHA＜28% extracted after 4 hours, and post is pressed and carried to 18.0MPa, obtain being rich in the product of DHA, DHA＞64%, EPA＜10%, be rich in EPA product 270 grams, be rich in DHA product 95 grams, total recovery is up to 91%.

Get fish oil 50 grams that are rich in DHA or EPA, β-CO cyclodextrin 10 restrains, ethyl cellulose 10 grams, and starch 10 grams, nor-pair of hydrogen guaiaretic acid 0.1 restrains and correctives 0.2 gram, and other are together

Embodiment 1.

Claims

1. slow-releasing concentrated fish oil sheet is characterized in that comprising each component of following weight ratio: fish oil 50, clathrate β-CD, ring aleurone 2-10, slow releasing tablet ethyl cellulose 5-10, excipient starch 5-10, the two hydrogen of the lucky methyl of antioxidant are more made wood acid 0.05-0.1, correctives 0.1-0.2.

2. the method for making of fish oil slow releasing tablet as claimed in claim 1 is characterized in that using earlier CO ₂The method of super critical extracting and rectifying makes the fish oil that contains a high proportion of DHA/EPA of high concentration, again fish oil and above-mentioned each component are mixed, make effective ingredient fish oil generation enclose, curing, stable, disperse, the mesh screen screening of reuse 0.9,60 ℃ dry down, augments the pelletize of 5-10 part Pulvis Talci, with the screening of 3.6mm mesh screen, drying is 1 hour under 60 ℃, and powder is pressed into the tablet or the pill of 0.5-1 gram/sheet.

3. method for making as claimed in claim 2 is characterized in that described CO ₂The super critical extracting and rectifying parameter is: extraction temperature 34-38 ℃, pressure 11-14MPa, rectification pressure are 11-14MPa, 1 section column temperature 37-39 ℃, 2 sections column temperature 42-44 ℃, 3 sections column temperature 47-49 ℃, 4 sections column temperature 52-54 ℃, separation temperature 40-45 ℃, pressure is 6.0-6.5MPa.