CN101416997B - Preparation technique of bitter melon powder and cucumber powder - Google Patents

Preparation technique of bitter melon powder and cucumber powder Download PDF

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CN101416997B
CN101416997B CN2007101634790A CN200710163479A CN101416997B CN 101416997 B CN101416997 B CN 101416997B CN 2007101634790 A CN2007101634790 A CN 2007101634790A CN 200710163479 A CN200710163479 A CN 200710163479A CN 101416997 B CN101416997 B CN 101416997B
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filtrate
momordicae charantiae
fructus momordicae
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mirabilitum
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CN101416997A (en
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邹准
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Abstract

The invention provides a method for preparing a balsam pear cream or a cucumber cream. The method comprises the following steps: the balsam pear and/or the cucumber are/is squeezed or extracted, filtered and the squeezed or extracted filtrate obtained is divided into two parts: a filtrate 1 accounting for 60 percent to 65 percent (volume) and a filtrate 2 accounting for 35 percent to 40 (volume); the filtrate 2 is added with mirabilite or mirabilite and 1 time to 8 times of water (optional), stirring is carried out to dissolve the mirabilite, heating, filtration, concentration and cream drainage are carried out, thus obtaining a balsam pear cream or cucumber cream crude product 1 and a mother liquid 1; concentration and cream drainage are conducted to the mother liquid 1 to obtain a balsam pear cream and/or cucumber cream crude product 2; and the filtrate 1 is filtered and added with the balsam pear cream or the cucumber cream crude product 1 and/or the balsam pear cream and/or cucumber cream crude product 2, the mixture is stirred to dissolve the crude products, heated, filtered and concentrated and then cream drainage or direct drying is conducted, thus obtaining the balsam pear cream and/or cucumber cream final product. The balsam pear cream and/or the cucumber cream have/has high yields, high purity and low pesticide content, meet/meets the hygienic standard of China with controllable quality and accurate curative effect, and the curative effect is similar to that of traditional creams.

Description

The preparation method of a kind of Fructus Momordicae charantiae cremor or HUANGGUASHUANG
Technical field
The present invention relates to a kind of Chinese medicine preparation technology, specifically, the present invention relates to the system method of a kind of Fructus Momordicae charantiae cremor or HUANGGUASHUANG, belong to field of traditional Chinese medicine pharmacy.
Background technology
Fructus Momordicae charantiae cremor is a kind of medication among the people, ancient literature is not seen and is recorded, and is stated from " Hunan Chinese crude drug concocted specification ", is the converted products of Fructus Momordicae charantiae and Natrii Sulfas, its preparation method: Natrii Sulfas filled in hang on the shady and cool ventilation place in the Fructus Momordicae charantiae, collect " frost " that ooze out formation and be Fructus Momordicae charantiae cremor.Perhaps mix with Natrii Sulfas with Fructus Momordicae charantiae chopping, the yellow sand cylinder of packing into, with cylinder cap good after, place the ventilation, after a couple of days, the adularescent Refined Mercurous chloride is separated out outside the yellow sand cylinder, is Fructus Momordicae charantiae cremor.Fructus Momordicae charantiae cremor, salty in the mouth, little bitterness are trembled with fear; GUIXIN, spleen, stomach, large intestine channel have heat clearing away and internal heat reducing, and the effect of removing toxic substances and promoting subsidence of swelling is used for laryngopharynx swelling and pain, aphtha of the mouth and tongue, tonsillitis sore throat, the acute catarrhal conjunctivitis swelling pain; Miliaria, skin ulcer is swollen, swelling and pain of hemorrhoid etc.
Application number is the preparation method that discloses a kind of Fructus Momordicae charantiae cremor among the 02132820.X, and its step is as follows: a, get bright Fructus Momordicae charantiae; B, clean with clear water; C, bright Fructus Momordicae charantiae go flesh, chopping; D, get sodium sulfate; E, the bright Fructus Momordicae charantiae that step c is obtained mix with sodium sulfate, heating and refluxing extraction 2~6 hours; F, filtration; G, secondary concentration crystallization; H, air slaking, drying; Among the step a in bright Fructus Momordicae charantiae and the steps d weight ratio of sodium sulfate be followed successively by: (80~150): (15~40).
Application number is the preparation method that discloses a kind of Fructus Momordicae charantiae cremor among the 02145017.X: get clean ripe bright Fructus Momordicae charantiae, draw out seed core, the Natrii Sulfas of in abdomen, packing into, collect white crystalline powder, dissolve white crystalline powder with water for injection, cooling, filtration, concentrating under reduced pressure, crystallization are with the dried Fructus Momordicae charantiae cremor that promptly gets of wind.
02145017.X in disclosed preparation method be traditional, openly be the preparation method that extracts earlier post crystallization among the 02132820.X.This class methods operation is simple and crude, and product quality is wayward, and purity is not high, and vulnerable to pollution has high input, and yields poorly, and difficulty reaches medicinal standard.
HUANGGUASHUANG also is a kind of medication among the people, and method for making is similar with Fructus Momordicae charantiae cremor or identical.The HUANGGUASHUANG salty in the mouth, cold in nature; Return spleen, stomach, large intestine channel, have heat clearing away and internal heat reducing, the effect of removing toxic substances and promoting subsidence of swelling is used for laryngopharynx swelling and pain, aphtha of the mouth and tongue, acute catarrhal conjunctivitis swelling pain; Acne, skin ulcer are swollen, miliaria etc.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG, Fructus Momordicae charantiae cremor of being made and/or HUANGGUASHUANG yield height, purity height, Fructus Momordicae charantiae or Fructus Cucumidis sativi active constituent content height, agricultural residual content are low, meet state health standards, quality controllable, favorable reproducibility, suitable large-scale industrial production, determined curative effect in the use is with the white curative effect no significant difference of tradition.
To achieve these goals, the technical solution used in the present invention is as follows:
The preparation method of a kind of Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG is characterized in that, described preparation method may further comprise the steps:
(1) Fructus Momordicae charantiae and/or Fructus Cucumidis sativi are cleaned, broken, squeeze the juice, perhaps water and/or at least a medicinal organic solvent extract, and filter, and the filtrate of squeezing or extracting of gained is divided into two parts, the volume of filtrate 1 accounts for 60%~65% of total filtrate, and the volume of filtrate 2 accounts for 35%~40% of total filtrate;
(2) add RUPIXIAO or Mirabilitum and water in filtrate 2, heating and stirring make its dissolving, filter, and crystallization behind the concentrated filtrate obtains Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 1 and mother solution 1;
(3) mother solution 1 is concentrated the back crystallization, obtain Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 2;
(4) Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 1 and Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 2 are joined in the filtrate filtered 1, heating is also stirred and is made its dissolving, filters the back concentrated filtrate, and crystallization or convection drying obtain Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG finished product.
Also the Mirabilitum in the above-mentioned steps directly can be dissolved in the water earlier, filter then its filtrate is mixed with the extraction filtrate of Fructus Momordicae charantiae and/or Fructus Cucumidis sativi, as follows:
A, with Fructus Momordicae charantiae or Fructus Cucumidis sativi clean, broken, squeeze the juice, perhaps extract with water extraction or medicinal organic solvent, with squeezing or extracting liq centrifugal filtration of gained, obtain the filtrate of Fructus Momordicae charantiae or Fructus Cucumidis sativi.
B, Mirabilitum is dissolved in the water, the water yield is controlled at and can makes the dissolved scope of Mirabilitum, stirs to make the Mirabilitum dissolving under 35~60 ℃ of conditions, and centrifugal filtration obtains Mirabilitum filtrate.
C, the filtrate of Fructus Momordicae charantiae or Fructus Cucumidis sativi and Mirabilitum filtrate are mixed, filter, under 60~70 ℃ of conditions, be evaporated to 1.15~1.40g/cm 3, the gained concentrated solution is at the condition crystallization below 15 ℃, or spray drying, gets Fructus Momordicae charantiae cremor or HUANGGUASHUANG.
In the preparation method of the present invention, Fructus Momordicae charantiae and/or Fructus Cucumidis sativi can be cleaned, directly squeeze the juice after the fragmentation, also can the method with reference to Chinese medicine extraction adopt solvent to extract after fragmentation, solvent wherein can be one of water, medicinal organic solvent or two kinds or two or more mixing.Directly squeeze the juice and can not destroy effective ingredient in Fructus Momordicae charantiae and the Fructus Cucumidis sativi; Solvent extracts and to be generally reflux, extract,, the effective ingredient in Fructus Momordicae charantiae and the Fructus Cucumidis sativi fully can be dissolved in the solvent, and be easy to filter and wait processing, adopts the medicinal solvent of low boiling among the present invention, can protect the effective ingredient in the raw material well.
Water or medicinal organic solvent that being extracted as in the described step (1) adopted Fructus Momordicae charantiae and/or 1~8 times of weight of Fructus Cucumidis sativi extract the water of preferred 2~5 times of weight or medicinal organic solvent.
The weight proportion of described Fructus Momordicae charantiae and/or Fructus Cucumidis sativi and Mirabilitum or Natrii Sulfas or sodium sulfate is: 1~15; Preferred Fructus Momordicae charantiae and Mirabilitum weight proportion are: 100: 25, Fructus Cucumidis sativi and Mirabilitum proportioning were 100: 27.
In the step of described preparation method (2), when step (1) is to squeeze the juice to obtain filtrate, perhaps extract with medicinal organic solvent, or but the amount of water extraction water is when insufficient, in filtrate 2, add an amount of water, the water that adds can improve the dissolving quality and the dissolution velocity of Mirabilitum or Natrii Sulfas or sodium sulfate, reduce dissolution time, the consumption of water is add Mirabilitum or Natrii Sulfas or sodium sulfate weight 1~8 times, the consumption of water is add Mirabilitum or Natrii Sulfas or sodium sulfate weight 1~8 times among the step B, and the consumption of preferred water is the weight of 2.5~6 times of Mirabilitums or Natrii Sulfas or sodium sulfate.
Being heated to be described in the step of described preparation method (2) is heated to 35~60 ℃, after the centrifugal filtration, is evaporated to 1.15~1.40g/cm under 40~70 ℃ condition 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor or HUANGGUASHUANG crude product 1 and mother solution 1.
Simmer down in the step of described preparation method (3): mother solution 1 is evaporated to 1.15~1.40g/cm under 40~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 2.
In the step of described preparation method (4), described filtration back concentrated filtrate is: be evaporated to 1.15~1.40g/cm under 40~70 ℃ condition 3, described crystallization is with concentrated solution crystallization under the condition below 15 ℃.
Described medicinal organic solvent is respectively: one of ethanol, methanol, ether, acetone, chloroform, ethyl acetate, dichloroethanes or its mixture.
Filtration treatment among the present invention adopts the filter method that is fit to prior art of the present invention, as centrifugal filtration, diatomite filtration, ultrafiltration, nanofiltration etc.
Wherein said concentration adopts and is fit to method for concentration of the prior art of the present invention, as concentrating under reduced pressure etc.
Wherein said dried adopts the drying means that is fit to prior art of the present invention, as bake drying, spray drying, lyophilization etc.
Mirabilitum is the natural minerals of contains sodium sulfate, through the refining crystalline solid that forms.Because of processing difference, Mirabilitum is arranged, Natrii Sulfas, the branch of Matrii Sulfas Exsiccatus has the repercussive of relieving inflammation or internal heat effect, the kind conjunctival congestion and swelling pain of controlling, swelling throat is mashed, skin infection, acute mastitis, hemorrhoid, diseases such as acute appendicitis.Mirabilitum described in the present invention also can be the mixture of a kind of of Natrii Sulfas, Matrii Sulfas Exsiccatus, sodium sulfate or at least two kinds.
Fructus Momordicae charantiae of the present invention (Momordica charantiap) source is the fruit of cucurbitaceous plant Fructus Momordicae charantiae.Nature and flavor: bitter, cold, composition: the main Charantin, albuminoid active substance (being α-Charantin, β-Charantin, MAP30), insulin-like activity substance of containing (is polypeptide-P) and several amino acids.Function: the clearing away summer-heat heat clearing away, make eye bright, detoxify.Control calentura, heatstroke, dysentery, acute conjunctivitis pain, the erysipelas that swells and ache, malignant boil.Described Fructus Cucumidis sativi (Cucumisativus) Cucurbitaceae, Cucumis.Another name, cucumber, Herba Cynanchi Corymbosi, Fructus Trichosanthis Cucumeroidis.Flavor efficacy: cool in nature, sweet in the mouth; Go into lung, stomach, large intestine channel.Effect cures mainly: clearing away heat and promoting diuresis, removing toxic substances and promoting subsidence of swelling, promoting the production of body fluid to quench thirst.Cure mainly the fever of the body excessive thirst, laryngopharynx swelling and pain, wind heat ophthalmic, jaundice due to damp-heat, diseases such as dysuria.Contain micro-vitamin C, carotene, hydroxymalonic acid, Fructus Cucumidis sativi oil, cucurbitacin C, chlorogenic acid, cucumber chitinase in the Fructus Cucumidis sativi, reach needed by human nutrients such as a small amount of saccharide, protein, calcium, phosphorus, ferrum.
Prove that through chemical analysis similar to existing Fructus Momordicae charantiae cremor or HUANGGUASHUANG chemical constituent by Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG that preparation method of the present invention makes, steady quality meets the national drug standards; Through pharmacodynamics test, compare there was no significant difference with existing Fructus Momordicae charantiae cremor or HUANGGUASHUANG in Fructus Momordicae charantiae cremor or HUANGGUASHUANG that preparation method of the present invention aspect the anti-inflammatory, antibacterial effect makes.
Preparation method of the present invention, with short production cycle, shorten to 2 days by 20 days of traditional handicraft; Yield height (in sodium sulfate), yield is 85~95%, is 10~35 times of existing preparation process recovery ratio; Cost is low, and per ton cost reduces more than 20,000 yuan, can reduce by 50~80% than existing processes; Do not have " three wastes " and pollute, favorable reproducibility is fit to large-scale industrial production.
Description of drawings
Fig. 1, Fig. 2 are the process charts that the present invention prepares.
The specific embodiment
Following embodiment further describes the present invention, but described embodiment only is used to illustrate the present invention rather than restriction the present invention.
Embodiment 1
Get Fructus Momordicae charantiae 100kg, with its clean, broken, with 400 L, 75% alcohol reflux 1 hour, centrifugal filtration, with the filtrate separated into two parts: filtrate 1 accounts for 65% of total filtrate volume, and filtrate 2 accounts for 35% of total filtrate volume; In filtrate 2, add 25kg Mirabilitum and 60 L water, can make Natrii Sulfas stirring and dissolving under 50 ℃ condition, after the centrifugal filtration, filtrate is evaporated to d:1.30g/cm under 60~62 ℃ 3,, obtain Fructus Momordicae charantiae cremor crude product 1 and mother solution 1 again at crystallization below 15 ℃; Mother solution 1 is evaporated to d:1.3g/cm under 60~62 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 2 again; Fructus Momordicae charantiae cremor crude product 1 and Fructus Momordicae charantiae cremor crude product 2 are added in the filtrate 1, are heated to 45 ℃ of following stirring and dissolving, filter back concentrating under reduced pressure d:1.3g/cm under 58~60 ℃ of conditions 3, crystallization, obtain the Fructus Momordicae charantiae cremor finished product.The yield of Fructus Momordicae charantiae cremor (in sodium sulfate) is 94%.
Embodiment 2
Get Fructus Momordicae charantiae 20kg, it is cleaned broken, with 20 L75% alcohol reflux 1 hour, centrifugal filtration, with the filtrate separated into two parts of gained: filtrate 1 accounts for 60% of total filtrate volume, and filtrate 2 accounts for 40% of total filtrate volume; In filtrate 2, add 20kg Natrii Sulfas and 160 L water, under 35 ℃ condition, stir and make the Natrii Sulfas dissolving, after the centrifugal filtration, under 68~70 ℃, be evaporated to d:1.40g/cm 3,, obtain Fructus Momordicae charantiae cremor crude product 1 and mother solution 1 at crystallization below 15 ℃; Mother solution 1 is evaporated to d:1..40g/cm under 68~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 2; To add Fructus Momordicae charantiae cremor crude product 1 and Fructus Momordicae charantiae cremor crude product 2 after filtrate 1 filtration, stirring and dissolving is heated to 35 ℃, filters under 52~54 ℃ of conditions in back to reduce pressure ConcentrateTo d:1..40g/cm 3, spray drying obtains the Fructus Momordicae charantiae cremor finished product.The yield of Fructus Momordicae charantiae cremor (in sodium sulfate) is 85%.
Embodiment 3
Get Fructus Momordicae charantiae 15kg, with its clean, broken, with 120 L water reduced-pressure backflows 1 hour, centrifugal filtration, with the filtrate separated into two parts of gained: filtrate 1 accounts for 65% of total filtrate volume, and filtrate 2 accounts for 35% of total filtrate volume; In filtrate 2, add 0.6kg Mirabilitum and 0.4kg Natrii Sulfas, under 60 ℃ condition, stir and make Mirabilitum and Natrii Sulfas dissolving, after the ultrafiltration, under 68~70 ℃ condition, be evaporated to d:1.25g/cm 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 1 and mother solution 1; Mother solution 1 is evaporated to d:1.25g/cm under 68~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 2; Filtrate 1 is filtered the back add Fructus Momordicae charantiae cremor crude product 1 and Fructus Momordicae charantiae cremor crude product 2, stirring and dissolving is filtered, and is evaporated to d:1.25g/cm under 68~70 ℃ condition 3, the concentrated solution lyophilization obtains the Fructus Momordicae charantiae cremor finished product.Fructus Momordicae charantiae cremor yield (in sodium sulfate) is 92%.
Embodiment 4
Get Fructus Momordicae charantiae 80kg, with its clean, broken, squeeze the juice, filter, gained squeezed the filtrate separated into two parts: filtrate 1 and filtrate 2, filtrate 1 accounts for 60% of total filtrate volume, filtrate 2 accounts for 40% of total filtrate volume; In filtrate 2, add 20kg Matrii Sulfas Exsiccatus and 80L water, under 45 ℃ condition, stir and make the Matrii Sulfas Exsiccatus dissolving, behind the diatomite filtration, under 68~70 ℃ condition, be evaporated to d:1.3 g/cm 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 1 and mother solution 1; Mother solution 1 is evaporated to d:1.35g/cm under 68~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains HUANGGUASHUANG crude product 2; Fructus Momordicae charantiae cremor crude product 1 and Fructus Momordicae charantiae cremor crude product 2 are joined in the filtrate 1, make its stirring and dissolving, filter, under 68~70 ℃ condition, be evaporated to d:1.35g/cm 3, concentrated solution is crystallization under the condition below 15 ℃, obtains the Fructus Momordicae charantiae cremor finished product.Fructus Momordicae charantiae cremor yield (in sodium sulfate) is 86%.
Embodiment 5
Get Fructus Cucumidis sativi 100kg, with its clean, broken, with 400 L, 75% alcohol reflux 1 hour, centrifugal filtration, with the filtrate separated into two parts: filtrate 1 accounts for 65% of total filtrate volume, and filtrate 2 accounts for 35% of total filtrate volume; In filtrate 2, add 25kg Mirabilitum and 70L water, can make Natrii Sulfas stirring and dissolving under 50 ℃ condition, after the centrifugal filtration, filtrate is evaporated to d:1.30g/cm under 60-62 ℃ 3,, obtain Fructus Momordicae charantiae cremor crude product 1 and mother solution 1 again at crystallization below 15 ℃; Mother solution 1 is evaporated to d:1.30g/cm under 60~62 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 2 again; Fructus Momordicae charantiae cremor crude product 1 and Fructus Momordicae charantiae cremor crude product 2 are added in the filtrate 1, are heated to 45 ℃ of following stirring and dissolving, filter the back and under 48~50 ℃ of conditions, be evaporated to d:1.30g/cm 3, crystallization, obtain the Fructus Momordicae charantiae cremor finished product.The yield of HUANGGUASHUANG (in sodium sulfate) is 95%.
Embodiment 6
Get Fructus Cucumidis sativi 10kg and Fructus Momordicae charantiae 10kg, with its clean, broken, with 20 L, 75% alcohol reflux 1 hour, centrifugal filtration, with the filtrate separated into two parts of gained: filtrate 1 accounts for 60% of total filtrate volume, and filtrate 2 accounts for 40% of total filtrate volume; In filtrate 2, add 20kg Natrii Sulfas and 160 L water, under 35 ℃ condition, stir and make the Natrii Sulfas dissolving, after the centrifugal filtration, under 68~70 ℃, be evaporated to d:1.20g/cm 3,, obtain Fructus Cucumidis sativi and Fructus Momordicae charantiae cremor crude product 1 and mother solution 1 at crystallization below 15 ℃; Mother solution 1 is evaporated to d:1.40g/cm under 68~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Cucumidis sativi and Fructus Momordicae charantiae cremor crude product 2; With adding Fructus Cucumidis sativi and Fructus Momordicae charantiae cremor crude product 1 and Fructus Cucumidis sativi and Fructus Momordicae charantiae cremor crude product 2 after filtrate 1 filtration, be heated to 35 ℃ of stirring and dissolving,, filter the back and under 55~57 ℃ of conditions, be concentrated into d:1.40g/cm 3, spray drying obtains Fructus Cucumidis sativi and Fructus Momordicae charantiae cremor finished product.The yield of Fructus Cucumidis sativi and Fructus Momordicae charantiae cremor (in sodium sulfate) is 87%.
Embodiment 7
Get Fructus Cucumidis sativi 15kg, with its clean, broken, with 120 L water reduced-pressure backflows 1 hour, centrifugal filtration, with the filtrate separated into two parts of gained: filtrate 1 accounts for 65% of total filtrate volume, and filtrate 2 accounts for 35% of total filtrate volume; In filtrate 2, add 1kg sodium sulfate, under 60 ℃ condition, stir and make the sodium sulfate dissolving, behind the nanofiltration, under 68~70 ℃ condition, be evaporated to d:1.20g/cm 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 1 and mother solution 1; Mother solution 1 is evaporated to d:1.20g/cm under 68~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 2; Filtrate 1 is filtered the back add Fructus Momordicae charantiae cremor crude product 1 and Fructus Momordicae charantiae cremor crude product 2, stirring and dissolving is filtered, and is evaporated to d:1.20g/cm under 68~70 ℃ condition 3, the concentrated solution lyophilization obtains the Fructus Momordicae charantiae cremor finished product.HUANGGUASHUANG yield (in sodium sulfate) is 90%.
Embodiment 8
Get Fructus Cucumidis sativi 80kg, with its clean, broken, squeeze the juice, filter, gained squeezed the filtrate separated into two parts: filtrate 1 and filtrate 2, filtrate 1 accounts for 60% of total filtrate volume, filtrate 2 accounts for 40% of total filtrate volume; In filtrate 2, add 20kg Matrii Sulfas Exsiccatus and 80 L water, under 45 ℃ condition, stir and make the Matrii Sulfas Exsiccatus dissolving, after the centrifugal filtration, under 68~70 ℃ condition, be evaporated to d:1.15g/cm 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor crude product 1 and mother solution 1; Mother solution 1 is evaporated to d:1.15g/cm under 68~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains HUANGGUASHUANG crude product 2; Fructus Momordicae charantiae cremor crude product 1 and Fructus Momordicae charantiae cremor crude product 2 are joined in the filtrate 1, make its stirring and dissolving, filter, under 68~70 ℃ condition, be evaporated to d:1.15g/cm 3, concentrated solution is crystallization under the condition below 15 ℃, obtains the Fructus Momordicae charantiae cremor finished product.HUANGGUASHUANG yield (in sodium sulfate) is 85%.
Embodiment 9
Get Fructus Momordicae charantiae 100kg, with its clean, broken, squeeze the juice, with gained squeeze liquid centrifugal filtration, obtain the filtrate of Fructus Momordicae charantiae; The 25kg Mirabilitum is dissolved in the 100L water, stir under 60 ℃ of conditions and make the Mirabilitum dissolving, centrifugal filtration obtains Mirabilitum filtrate; The filtrate and the Mirabilitum filtrate of Fructus Momordicae charantiae are mixed, filter, under 68~70 ℃ of conditions, be evaporated to 1.35g/cm 3, the gained concentrated solution gets the Fructus Momordicae charantiae cremor finished product at the condition crystallization below 15 ℃.Fructus Momordicae charantiae cremor yield (in sodium sulfate) is 95%.
Embodiment 10
Get Fructus Momordicae charantiae 15kg, clean, broken,,, obtain the filtrate of Fructus Momordicae charantiae the extracting liq centrifugal filtration of gained with 120 L water reduced-pressure backflows 1 hour; The 1kg Natrii Sulfas is dissolved in the 1L water, stir under 35 ℃ of conditions and make the Natrii Sulfas dissolving, centrifugal filtration obtains Natrii Sulfas filtrate; The filtrate and the Natrii Sulfas filtrate of Fructus Momordicae charantiae are mixed, filter, under 60~62 ℃ of conditions, be evaporated to 1.20g/cm 3, the lyophilization of gained concentrated solution gets the Fructus Momordicae charantiae cremor finished product.Fructus Momordicae charantiae cremor yield (in sodium sulfate) is 86%.
Embodiment 11
Get Fructus Cucumidis sativi 100kg, clean, broken, squeeze the juice, with gained squeeze liquid centrifugal filtration, obtain the filtrate of Fructus Cucumidis sativi; The 50kg Mirabilitum is dissolved in the 120L water, stir under 60 ℃ of conditions and make the Mirabilitum dissolving, centrifugal filtration obtains Mirabilitum filtrate; Filtrate and the Mirabilitum filtrate of Fructus Cucumidis sativi are mixed, filter, under 65~67 ℃ of conditions, be evaporated to 1.40g/cm 3, the gained concentrated solution gets the HUANGGUASHUANG finished product at the condition crystallization below 15 ℃.HUANGGUASHUANG yield (in sodium sulfate) is 87%.
Embodiment 12
Get Fructus Cucumidis sativi 100kg, with its clean, broken, with 400 L, 75% alcohol reflux 1 hour,, obtain the filtrate of Fructus Cucumidis sativi with the extracting liq centrifugal filtration of gained; The 27kg Mirabilitum is dissolved in the 100 L water, stir under 45 ℃ of conditions and make the Mirabilitum dissolving, centrifugal filtration obtains Mirabilitum filtrate; Filtrate and the Mirabilitum filtrate of Fructus Cucumidis sativi are mixed, filter, under 60~62 ℃ of conditions, be evaporated to 1.15g/cm 3, gained concentrated solution spray drying gets the HUANGGUASHUANG finished product.HUANGGUASHUANG yield (in sodium sulfate) is 92%.
Embodiment 13~18, it is Fructus Momordicae charantiae and/or Fructus Cucumidis sativi are extracted in drug of choice of the present invention with the mixed liquor of organic solvent methanol, dichloroethanes, acetone, ethyl acetate, chloroform and ether and ethyl acetate instantiation, except that extraction solvent changes, preparation method and other conditions are all with of the present invention described consistent, for details see attached table:
Subordinate list:
Embodiment number Solvent The weight of Fructus Cucumidis sativi/Fructus Momordicae charantiae The solvent volume The weight of Mirabilitum Step (2) adds the volume of water Temperature in the step (2) The concentrating under reduced pressure temperature Product yield
13 Methanol Fructus Momordicae charantiae 100kg 400L 25kg 60L 50℃ 40~42℃ 94%
14 Dichloroethanes Fructus Cucumidis sativi 15kg 120L 1kg 8L 35℃ 42~44℃ 85%
15 Acetone Fructus Cucumidis sativi 50kg 50L 50kg 120L 60℃ 48~50℃ 88%
16 Ethyl acetate Fructus Momordicae charantiae 50kg 50L 10kg 50L 40℃ 56~58℃ 90%
17 Chloroform Fructus Momordicae charantiae 50kg 100L 50kg 150L 45℃ 52~54℃ 86%
18 Ethyl acetate and ether Fructus Cucumidis sativi 100kg 200L 27kg 120L 40℃ 42~44℃ 95%

Claims (13)

1. the preparation method of Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG is characterized in that described preparation method may further comprise the steps:
(1) Fructus Momordicae charantiae and/or Fructus Cucumidis sativi are cleaned, broken, squeeze the juice, perhaps water and/or at least a medicinal organic solvent extract, filter, it is 60%~65% filtrate 1 and filtrate 2 two parts of 35%~40% that the filtrate of squeezing the juice or extracting of gained is divided into weight percentage;
(2) add RUPIXIAO or Mirabilitum and water in filtrate 2, stir and make the Mirabilitum dissolving, heating is filtered, and crystallization behind the concentrated filtrate obtains Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 1 and mother solution 1;
(3) mother solution 1 is concentrated the back crystallization, obtain Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 2;
(4) Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 1 and Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 2 are joined in the filtrate filtered 1, heating and stirring and dissolving are filtered the back concentrated filtrate, and crystallization or convection drying obtain Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG finished product.
2. the preparation method of Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG is characterized in that described preparation method may further comprise the steps:
A, with Fructus Momordicae charantiae or Fructus Cucumidis sativi clean, broken, squeeze the juice, perhaps extract with water extraction or medicinal organic solvent, with squeezing or extracting liq centrifugal filtration of gained, obtain the filtrate of Fructus Momordicae charantiae or Fructus Cucumidis sativi;
B, Mirabilitum is dissolved in the water, the water yield is controlled at and can makes the dissolved scope of Mirabilitum, stirs to make the Mirabilitum dissolving under 35~60 ℃ of conditions, and centrifugal filtration obtains Mirabilitum filtrate;
C, the filtrate of Fructus Momordicae charantiae or Fructus Cucumidis sativi and Mirabilitum filtrate are mixed, filter, under 40~70 ℃ of conditions, be evaporated to 1.15~1.40g/cm 3, the gained concentrated solution is at the condition crystallization below 15 ℃, or direct spray drying after filtering, and gets Fructus Momordicae charantiae cremor or HUANGGUASHUANG.
3. preparation method according to claim 1 and 2 is characterized in that, water or organic solvent that being extracted as in described step (1) or the steps A adopted Fructus Momordicae charantiae and/or 1~8 times of weight of Fructus Cucumidis sativi extract.
4. preparation method according to claim 3 is characterized in that, the water or the organic solvent that are extracted as employing Fructus Momordicae charantiae and/or 2~5 times of weight of Fructus Cucumidis sativi in described step (1) or the steps A.
5. preparation method according to claim 1 and 2 is characterized in that, described Fructus Momordicae charantiae and/or Fructus Cucumidis sativi and Mirabilitum weight proportion are: 1-15.
6. preparation method according to claim 5 is characterized in that, described Fructus Momordicae charantiae and Mirabilitum weight proportion are: 100: 25, Fructus Cucumidis sativi and Mirabilitum proportioning were 100: 27.
7. preparation method according to claim 1 and 2 is characterized in that, in the step of described preparation method (2), when step (1) is to squeeze the juice to obtain filtrate, perhaps extract with medicinal organic solvent, add water in filtrate 2, the consumption of water is add 1~8 times of Mirabilitum weight; Among the step B of described preparation method that Mirabilitum is soluble in water, the consumption of water is 1~8 times of Mirabilitum weight.
8. preparation method according to claim 7 is characterized in that, in the step of described preparation method (2), when step (1) is to squeeze the juice to obtain filtrate, perhaps extracts with medicinal organic solvent, adds water in filtrate 2, and the consumption of water is the weight of 2.5~6 times of Mirabilitums.
9. preparation method according to claim 1 is characterized in that, being heated to be described in the step of described preparation method (2) is heated to 35~60 ℃, after the centrifugal filtration, is evaporated to 1.15~1.40g/cm under 40~70 ℃ condition 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor or HUANGGUASHUANG crude product 1 and mother solution 1.
10. preparation method according to claim 1 is characterized in that, the simmer down in the step of described preparation method (3): mother solution 1 is evaporated to 1.15~1.40g/cm under 40~70 ℃ of conditions 3, crystallization under the condition below 15 ℃ obtains Fructus Momordicae charantiae cremor and/or HUANGGUASHUANG crude product 2.
11. preparation method according to claim 1 and 2 is characterized in that, among step of described preparation method (4) or the step C, described filtration back concentrated filtrate is: be evaporated to 1.15~1.40g/cm under 40~70 ℃ condition 3, described crystallization is that described drying is a spray drying with concentrated solution crystallization under the condition below 15 ℃.
12. preparation method according to claim 1 and 2 is characterized in that, described medicinal organic solvent is one of ethanol, methanol, ether, acetone, chloroform, ethyl acetate, dichloroethanes or its mixture.
13. preparation method according to claim 1 and 2 is characterized in that, described Mirabilitum is the mixture of a kind of of Natrii Sulfas, Matrii Sulfas Exsiccatus, sodium sulfate or at least two kinds.
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CN1364611A (en) * 2001-12-01 2002-08-21 李昆 Watermelon frost and its preparing method
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CN1364611A (en) * 2001-12-01 2002-08-21 李昆 Watermelon frost and its preparing method
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