CN109481561A - A kind of aloe cassia seed capsule and preparation method thereof of energy relaxing bowels to lose weight - Google Patents

Abstract

The invention discloses a kind of aloe cassia seed capsule and preparation method thereof of energy relaxing bowels to lose weight, the material components and its weight proportion of the capsule are as follows: 50-70 parts of plant extracts, 10-20 parts of aloe powder, 15-25 parts of dietary fiber, 3-8 parts of thickener, 8-13 parts of gelatin, 3-5 parts of plasticizer, 30-40 parts of pure water.

Description

A kind of aloe cassia seed capsule and preparation method thereof of energy relaxing bowels to lose weight

Technical field

The invention belongs to health product technology fields, relate generally to the aloe cassia seed capsule and its system of a kind of energy relaxing bowels to lose weight Preparation Method.

Background technique

Its unique closure property in view of soft capsule, can effectively guarantee the stabilization of content active constituent, also, by Soft capsule is widely used with portability in the dosage controllability that soft capsule has.Soft capsule, which removes, is applied to drug Outside, also it is widely used on many wholesome health foods.In recent years, from the point of view of the purpose for improving taking, even if pair The demand for not having water to be also easy to the chewable soft capsule taken increasingly improves.Disintegrating procedue is not present in chewable soft capsule, therefore Active ingredient draws are fast, especially suitable for child, the elderly and have the group for swallowing suffering.United States Patent (USP) US6280767 is disclosed A kind of chewable soft capsule, the soft capsule make capsule keep certain pliability by increasing the dosage of plasticizer, wherein rubber Gelatin in prescription: plasticizer=100: 100~600；U.S. Patent application US20050136104 discloses a kind of chewiness flexible glue Capsule, the soft capsule is by keeping higher moisture content that capsule is made to keep certain pliability, and wherein water content is up in rubber 27%；Chinese patent application 200910088218.6 discloses a kind of chewing soft capsule and preparation method thereof, which passes through One layer of sweet taste oxidant layer is precipitated outside soft capsule rubber and does not need chewing so that oral cavity directly contacts sweet taste oxidant layer when taking To experience sweet taste；Chinese patent ZL00806658.2 discloses a kind of masticatory pattern soft capsule for improving taking, in order to Increase mouthfeel when chewing, which sets room temperature in solid-like or semi-solid for soft capsule content, and inwardly The chocolate-based low melting point additive of tolerant middle addition, reduces the raw material smell of soft capsule rubber itself to a certain extent.

Cassia seed is legume cassia (Cassia obtusifolia L.) or little cassia tora (Cassia tora L.) Dry mature seed, for clinical conventional Chinese medicine and the natural plants of the dual-purpose of drug and food of the Ministry of Public Health, China promulgation.First recorded in " mind Agriculture book on Chinese herbal medicine warp ", nature and flavor are sweet, bitter, salty, slightly cold.Return liver, kidney, large intestine channel.With clearing liver and improving vision, the effect of relax bowel and defecation.Modern times grind Studying carefully proves that cassia seed has the pharmacological actions such as antibacterial, lowering blood pressure and blood fat, liver protection, diuresis.Cassia seed is derivative containing the awake class of a species of orchid, naphthalene A variety of chemical components such as object, carbohydrate, lipid, protein and microelement.In recent years in lipid-loweringing, the food of decompression, health food It is widely applied in natural drug.

Constipation (constipation) refers to that times of defecation caused by many reasons is reduced and excrement drying is difficult to resolve, including excrement Just dry discharge is unsmooth and excrement does not do also two kinds of situations of difficult discharge.It is mainly shown as that weekly defecation is no more than 2 times；At least 25% time occur defecation firmly less difficult defecation or defecation it is unsmooth；And often there are the swollen sense of rectum, exert oneself for a long time defecation, defecation A series of syndromes such as incomplete sense, abdominal distension abdominal pain.Constipation is one of digestive system common disease.Constipation often influences appetite and intestines The absorption of road nutriment makes internal noxious material in the extended residence time of enteron aisle, and is largely absorbed, and causes toxicity anti- It answers；Serious person can lead to acute myocardial infarction, cerebrovascular accident and threat to life.

Summary of the invention

To overcome the above-mentioned problems in the prior art, the present inventor provides by further investigation and a large number of experiments Following technical solution.

A kind of aloe cassia seed capsule of energy relaxing bowels to lose weight, the material component and its weight proportion of the capsule are as follows: plant 50-70 parts of extract, 10-20 parts of aloe powder, 15-25 parts of dietary fiber, 3-8 parts of thickener, 8-13 parts of gelatin, plasticizer 3-5 Part, 30-40 parts of pure water.The pure water need to be by pre-processing, i.e., by water used successively through Guartz filter, active carbon mistake Filter filtering, then by sodium ion exchange machine, then enter accurate filter filtering.

The thickener be one of starch, sodium alginate, Carmomer, pulullan polysaccharide, two or more The mixture of meaning ratio.

The plasticizer be one of glycerol, propylene glycol, sorbierite, polyethylene glycol, maltitol, two kinds or two kinds with The mixture of upper arbitrary proportion.

The material component and its weight proportion of the capsule are as follows: 50 parts of plant extracts, 10 parts of aloe powder, dietary fiber 15 Part, 3 parts of thickener, 8 parts of gelatin, 3 parts of plasticizer, 30 parts of pure water.

The material component and its weight proportion of the capsule are as follows: 70 parts of plant extracts, 20 parts of aloe powder, dietary fiber 25 Part, 8 parts of thickener, 13 parts of gelatin, 5 parts of plasticizer, 40 parts of pure water.

The material component and weight of the plant extracts are as follows: 5-10 parts of Semen Persicae extract, cassia seed extract 8-15 parts, 10-18 parts of angelica extract.

The purpose of the present invention is intended to provide a kind of pure Chinese medicine pharmaceutical composition capsule and preparation method thereof for defaecation, its energy The shortcomings that overcoming existing market existing procucts, and have effect it is good, it is highly-safe, have no toxic side effect, no dependence, quality stablize Controllably, easy to carry and take, the simple advantage of preparation process.

Pure Chinese medicine pharmaceutical composition capsule in the present invention is realized to adjust function of human body and improves functions of intestines and stomach, enhancing myenteron Tension, the effect for increasing intestines peristalsis.Wherein: in aloe big bitter Great Cold, settling downlink, main pharmacological is energy clearing stomach under rushing down Intestines cold and purgating heat and bowels, are the product of drastic purgation, record in such as " Bencao Jingshu ": " aloe it is cold can heat-clearing, hardship can purge heat eliminating dampness, bitter Can desinsection, to bitter to cold, therefore be the medicine except hot desinsection "；Cassia seed is conventional Chinese medicine, first recorded in Shennong's Herbal, nature and flavor are sweet, It is bitter, salty, slightly cold, return liver, large intestine channel, has effects that heat-clearing improving eyesight, sharp water defaecation.Cassia seed has multiple pharmacological effect, main Control the puckery pain of hot eyes, the more tears of photophobia, headache, dizziness, difficult urination, habitual constipation etc.；The fleece-flower root is bitter in taste, sweet, puckery, warm, returns Liver, kidney, the heart channel of Hang-Shaoyin, it is raw with having the effect of detoxifying, disappear carbuncle, relax bowel and defecation, it can be used for treating scrofula sore carbuncle, rubella itch, intestinal dryness Constipation, hyperlipemia；Oligofructose is a kind of natural active matter.It is to have to adjust intestinal flora, is proliferated Bifidobacterium, promotes The absorption of calcium, adjusts blood lipid, immunological regulation, and the novel sweetener of the healthcare functions such as anti-caries tooth was known as after the antibiotic epoch Most potential additive of new generation --- growth-promoting substance.Each raw material plays certain work all in terms of different to constipation With aloe, cassia seed are the primary raw material for improving gastrointestinal function, and it is movable to play the role of adjusting stomach and intestine；Assistant with oligofructose, The fleece-flower root, the gastrointestinal diseases such as adjuvant treatment diarrhea constipation.This formula can not only improve gastrointestinal function, treat constipation, moreover it is possible to Enhance immunity of organisms, has auxiliary therapeutic action to other diseases.Aloe, Liliaceae, aloe barbadensis Miller Aloe barbadensis Miller.Aloe property is bitter, cold, returns liver, stomach, large intestine channel." Chinese Pharmacopoeia " version one load in 2010 " is rushed down lower logical Just, clearing liver-fire, desinsection treat infantile malnutrition due to digestive disturbances or intestinalparasites.For constipation with heat retention ", " dictionary of medicinal plant " carries " heat-clearing, defaecation, desinsection.Control constipation with heat retention ".

Cassia seed, is leguminous plant, and Cassia Cassia obtusifalia L. or little cassia tora Cassia tora L.'s is dry Dry mature seed, be the Ministry of Public Health in 2002 announce in " notice about further specification healthy food material management " be both food Product are the Chinese medicine of drug again.Cassia seed is sweet, bitter, salty, slightly cold.Return liver, large intestine channel." Chinese Pharmacopoeia " 2010 editions loads are " clear Hot improving eyesight, relax bowel and defecation.For ... constipation "." dictionary of medicinal plant " carries " clearing liver, improving eyesight, Li Shui, defaecation.Control ... habit Inertia constipation ".

This standard is suitable for based on Semen Persicae extract, cassia seed extract, aloe powder, angelica extract, dietary fiber Raw material is wanted, through crushing, sieving, mixing, filling, packaging, is sterilized and the logical refreshing beauty of the manufactured Warner board with defaecation healthcare function Capsule product.This product functional component is Total saponin, barbaloin, insoluble diedairy fiber.

(1) quality examination of raw material

1, require material quality excellent, health must not be by pesticide, chemical substance, and poisonous metal and radioactive substance are dirty Dye must not contain the toxin being harmful to the human body.

2, the related standard of raw and auxiliary material buying strict implement, should there is the sanitary inspection qualification certificate in sourcing or the place of production.

3, workshop audits the quality inspection report of every kind of raw material, and confirmation can be used to produce when meeting the quality standard.

(2) production technology describes

1, it stocks up: Semen Persicae extract, cassia seed extract, aloe powder, angelica extract, dietary fiber being crushed, cross 80 Mesh, it is spare.

2, ingredient: each raw material is weighed by formula rate, mixing machine is put into and mixes well.

3, capsule is filling: mixed material being carried out to filling, No. 0 capsule on automatic capsule bottle placer, every contains content 0.45g。

4, capsule polishes: polishing on capsule polisher to canned capsule.

5, bottle: capsule is bottled (polyolefin plastics bottle), and every bottle.

6, pack: labelling is cased (corrugated case).

7, it irradiates: being irradiated with 60Co, dosage 6kGy.

8, examine storage: finished product is through after the assay was approved, being put in storage.

9, the cleanliness of 1~5 production environment is 100,000 grades, meets GB 17405-1998 requirement.

Compound basis

This product is using Semen Persicae extract, cassia seed extract, aloe powder, angelica extract, dietary fiber as primary raw material It is manufactured, prove that this product has the function of relax bowel and defecation through functional experiment.

Peach kernel: bitter in taste, sweet, flat.Return heart, liver, large intestine channel.With promoting blood circulation, the function of relax bowel and defecation.Health product is with work Blood and dissolving stasis power is strong, is used for blood stasis, postpartum stasis abdominal pain.Stir-baked SEMEN PERSICAE is relatively moisturized and blood, is chiefly used in dry constipation of intestines, abdominal distnetion It is full etc..

Cassia seed: it is bitter in taste, sweet, salty, it is slightly cold.Return liver, large intestine channel.With clearing liver and improving vision, the function of relax bowel and defecation.

Raw cassia seed is longer than removing heat from the liver, and ease constipation is dry.It is usually used in red eye, swell pain, constipation.The cold property rushed down of fried cassia subtracts It is weak, and fried effect can be improved, there is calming the liver to support the function of kidney.It can be used for having a headache, be dizzy, optic atrophy.

Aloe: Chinese medicine thinks that aloe has removing heat from the liver, defaecation.For constipation, infantile malnutrition, infantile convulsion；The diseases such as wet tinea are controlled outside Shape.Modern research suggests that it contains the chemical components such as barbaloin, aloin, protein.With antitumor, Digestive The effects of system, immune system, liver, cardiovascular system.

Radix Angelicae Sinensis: replenishing and activating blood, regulating menstruation and relieving pain, moistening intestines and relaxing bowels.For blood deficiency chlorosis, dizziness palpitaition, irregular menstruation, menostasis pain Through, asthenia cold abdominalgia, dry constipation of intestines, rheumatic arthralgia, injury from falling down, ulcer sores.Carbohydrate rich in, volatile component, ammonia Base acid, inorganic elements, have effect to the circulatory system, immune system, central nervous system impression, antitumor, gastrointestinal tract etc..

Dietary fiber: this product has important physiological function to human body, the final conclusion confirmed through a host of facts and research institute.Diet Fiber can be such that food shortens in the digestive tract by the time, generally account for about the 97% of total time in the residence time of big enteral, Food fiber makes the movement speed of the big enteral of material shorten 40%, and intestinal flora is made to change, and increases beneficial bacterium, and reduction has Evil bacterium, facilitates the wriggling of large intestine, increases defecation frequency, to have the function that prevent constipation.

A kind of aloe cassia seed capsule and preparation method thereof of energy relaxing bowels to lose weight, steps are as follows for the preparation method:

Step 1: raw material preparation；

Step 2: crushing；

Step 3: dry；

Step 4: sieving；

Step 5: mixing；

Step 6: dress capsule；

Step 7: packaging；

Step 8: irradiation sterilization.

The raw material preparation includes the preparation of plant extracts, specific as follows:

(1) preparation of Semen Persicae extract

Step (1) fresh peach kernel is carried out in far infrared sterilizer 90-120 seconds sterilize, 40-45 DEG C at a temperature of It is dried under reduced pressure 9-10h；The pressure being dried under reduced pressure is 0.001-0.05MPa；Then it carries out being dried under vacuum to aqueous 5-10%, institute again State vacuum drying in drying chamber carry out hot wind-it is infrared-microwave drying, 45-55 DEG C of hot blast temperature, far infrared radiation intensity 0.8-1W/cm², microwave heating first stage power is 100-150W, and second stage power is 200-300W, phase III power For 350-400W, conveyor belt speed 1-2m/min, recycle 9-10 times；It is stored in refrigerator after drying, storage temperature is -15 DEG C ~-10 DEG C；

The peach kernel of freezing is crushed to 100-200 mesh by step (2)；

The peach kernel of crushing is granulated by step (3), and the mean particle size after granulation is 2-4mm；

Raw material is placed in extraction kettle by step (4)；

Deionized deoxygenated water by preheating is injected into extraction with the flow velocity less than or equal to 100ml/min by step (5) In kettle；

Step (6) extraction；

Step (7) centrifugation: by extract liquor under the conditions of 2000-3000r/min, it is centrifuged 35-50min, takes supernatant；

Step (8) filtering: the supernatant obtained after centrifugation crosses micro-filtration bioceramic film, obtains filtrate, takes after precipitating Clear essential oil obtains peach kernel essential oil crude product；

Step (9) peach kernel essential oil crude product pours into the bottle for material of molecular distillation instrument and closes molecular distillation system and extraneous connection Logical all valves open condensed water, liquid nitrogen are added in cold-trap, and starting vacuum pump is de-gassed, until liquid level bubble-free is escaped Out；

Step (10) sets molecular distillation evaporating surface temperature as 30-50 DEG C, vacuum degree 200-700Pa, to temperature with Vacuum degree opens inlet valve when reaching setting value, adjusting feed flow rate is 1-3mL, revolving speed is to carry out after 200-400r/min deaerates The molecular distillation of crude essential oil, that collects heavy constituent purifying concentrated oil evaporates excess, obtains Semen Persicae extract, through detecting, wherein Amino acid and vitamin content are 60-70 weight %.

The micro-filtration bioceramic membrane filtration, the bioceramic film are oxidation zirconium base nano inorganic film, retention Molecular weight is 1500MW, and micro-filtration temperature is 20-25 DEG C；The nano inorganic film with a thickness of 10-15 microns；The nanometer nothing The material component and weight proportion of machine film are as follows: 3-5 parts of silica, 17-25 parts of rice hull ash, stabilized with yttrium oxide zirconium oxide 1- 3 parts, 4-8 parts of titanium carbide, 10-15 parts of carbon fiber, 1-3 parts of BeO, 1-3 parts of magnesium nitride, 3-4 parts of silicon carbide, Sc₂O₃4-8 parts；

It is extracted using ultrasound-enhanced subcritical water, including control system part, operating system part and ultrasound-enhanced Part is connected by the way of electric signal between control system part and operating system part.The Subcritical Water Extraction method, Under the conditions of 1-5MPa, 70-80 DEG C, the extraction of 30-60min is carried out to the substance in reaction kettle, then separates the object in reaction kettle Matter.

(2) preparation of cassia seed extract

Step 1: cassia seed is cleaned, dry, be crushed to 3cm-6cm, the weight ratio of cassia seed material and water is 1:(2.5- 3) it is put into progress high temperature and pressure extraction in cooker, obtains cassia seed juice and cassia seed slag；Boiling is extracted: cassia seed is in cooker In Extracting temperature be 125-130 DEG C, extraction time 120-180min；Cassia seed juice after extraction is passed through to the mistake of 100 mesh Step 2 cassia seed juice purification processes are carried out after strainer filtering, and cassia seed slag is delivered to step 3 workshop section and carries out ultra-fine cassia seed Ground-slag production.

Step 2: cassia seed juice obtained in step 1 is carried out purification processes, in turn include the following steps, tubular type centrifugation Separation, ultrafiltration membrance filter, decoloration is deodorized, nanofiltration membrane is concentrated, centrifugal spray drying；

Wherein, tubular type is centrifugated: will be centrifuged at a high speed by filtered cassia seed juice, centrifuge speed is 5000-7000r/min, the degreasing cassia seed juice after centrifugation enter ultrafiltration membrance filter process；

Wherein, ultrafiltration membrance filter: being the ultrafiltration of 500-800 dalton with molecular cut off by obtained degreasing cassia seed juice Macromolecular substances in film filtering removal clear liquid, the membrane pressure of the ultrafiltration membrane are 1.5-2MPa, and ultrafiltrate temperature is 35 DEG C -45 DEG C； Subsequently into decoloration deodorization process；

Wherein, decoloration is deodorized: activated carbon is added into the clear liquid obtained after ultrafiltration membrance filter and carries out decoloration deodorization, it is living Property carbon additional amount be ultrafiltration membrance filter after cassia seed juice weight 5%-10%, by be added activated carbon after clear liquid be warming up to 85-95 DEG C, and keep the temperature 20-40min, 60 DEG C -70 DEG C are then cooled to, standing after 30min-60min by aperture is 0.2-0.5 μm multilayer film filter carry out carbonization treatment；Subsequently into nanofiltration membrane enrichment process

Wherein, nanofiltration membrane is concentrated: the clear liquid of carbonization treatment is removed greatly with the nanofiltration membrane that aperture is divided into 200-300 dalton Partial moisture and inorganic salts, it is 20%-30% that clear liquid, which is concentrated into solid content, and the membrane pressure of the nanofiltration membrane is 1- 1.5MPa, nanofiltration temperature are 25 DEG C -40 DEG C；Subsequently into centrifugal spray dryer drying process；

Wherein, centrifugal spray drying: by the cassia seed juice by concentration through centrifugal spray drying tower drying, drying process In inlet temperature be 180 DEG C -190 DEG C, outlet temperature be 75 DEG C -85 DEG C.

(3) preparation of angelica extract

Step (1) cleans Radix Angelicae Sinensis, removes impurity, carries out 10-30 seconds in far infrared sterilizer, then carry out height again Temperature sterilizing sets sterilising temp range as 120-130 DEG C, and pressure is 0.2~0.3MPa, and sterilizing duration range is 30-40 minutes； Radix Angelicae Sinensis is placed in water and impregnate 1-24 hours, its water content is made to reach 30-50%；Radix Angelicae Sinensis after vacuum drying is broken in ultra micro Wall pulverizer is crushed to 400 mesh or more；Again into smashed Chinese Angelica Root, it is added 15-25 times of Chinese Angelica Root weight (g:ml) Ethyl alcohol, the concentration of the ethyl alcohol is 60-80 volume %, then passes through ultrasonic continuous stream biomixer, supersonic frequency 15- 40KHz, power 1000-3000W, flow is 15Kg, obtained broken Chinese Angelica Root suspension, PH=to suspension per hour 7；

Step (2) prepares angelica extract and filters；

After the evaporation of step (3) filtrate, resulting filtering extracting solution is the hydrosol ingredient extracted from Radix Angelicae Sinensis.

Step (4) collects distillate and obtains hydrosol, wherein collecting distillate is reverse osmosis treatment, the reverse osmosis trapped fluid of gained For the hydrosol of concentration, during reverse osmosis treatment, the membrane stack pressure of reverse osmosis membrane is 5-8MPa；The reverse osmosis treatment uses Reverse osmosis membrane desalination rate be 99.8%.

Step (2), which is specifically included, is concentrated above-mentioned angelica extract using vacuum suction method, and the temperature of vacuum suction concentration is 50-80 DEG C, time 1-3h, PH=7, the adsorbent of vacuum suction concentration is active carbon or non-polar macroporous resin, weight It is 3-4 times of former Radix Angelicae Sinensis weight, using the high volatile component extracted out when adsorbent Adsorption Concentration with gaseous state ethyl alcohol, gaseous state ethyl alcohol is then It is adsorbed the subsequent cool trap recycling of agent；Specially to be extracted by 75 volume % alcohol heat reflux, then be passed through when being classified as raw material D101 macroporous resin enrichment collects 95% alcohol-water and elutes position, continue silica gel after the elution removal of impurities of 75 volume % alcohol-waters Column chromatography, through methylene chloride: after methanol=13:3 elution removal of impurities, collecting methylene chloride: methanol=8:3 eluted fraction, remove molten The Radix Angelicae Sinensis hydrosol extract is obtained after agent；Using the Radix Angelicae Sinensis hydrosol extract as raw material, high performance liquid preparative chromatography is used (pHPLC) it is isolated and purified

Step (3) specifically includes, and pHPLC condition is as follows: ODS prepares chromatographic column；Eluent uses 50-60% methanol-water Add the formic acid or trifluoroacetic acid of 0.1-0.5% in 0-60min gradient elution, eluent；It is concentrated under reduced pressure after removal solvent to obtain the final product Radix Angelicae Sinensis hydrosol ingredient.

In the soaking process in the step (1), the vacuum pump connecting with closed container is opened, is extracted out in closed container Gas, the Radix Angelicae Sinensis valve in closed container is carried out vacuumizing dipping；Keep container inner pressure constant, 100-120 minutes, together When, in vacuum-pumping container, form ultrasonic activation；Ultrasonic power is 500W, ultrasonic time 5min；Stopping vacuumizes, extensive Air pressure in multiple closed container is atmospheric pressure, takes out the Radix Angelicae Sinensis by impregnating, spare.

Crushing in the step (1) includes the following steps:

Radix Angelicae Sinensis sealing after immersion is placed in constant temperature 1-2h in -15 to -10 DEG C of refrigerator, then takes out, it is cold to be placed in vacuum In lyophilizer, -40~-50 DEG C first are refrigerated to the cooling rate of 5-10 DEG C/min, 2-4h is kept, is then placed on Ku Wen again For cryostat 3h in -32~-36 DEG C of freezers, 400 mesh or more are crushed in super-micro wall-broken grinder.

Vacuum drying in the step (1) includes the Radix Angelicae Sinensis after the immersion that will be obtained, and it is red that hot wind-is carried out in drying chamber Outside-microwave drying, 50-65 DEG C of hot blast temperature, far infrared radiation intensity 0.5-0.75W/cm², microwave heating first stage power For 200-250W, second stage power is 250-350W, and phase III power is 300-200W, conveyor belt speed 1-2m/min, Circulation 3-4 times.

Filtering in the step (2) is by micro-filtration bioceramic membrane filtration；The bioceramic film is oxidation Zirconium-base nano inorganic thin film, molecular cut off 1500MW, micro-filtration temperature are 20-25 DEG C；Ultrafiltration retaining molecular weight is 400MW, ultrafiltrate temperature are 40 DEG C；The nano inorganic film with a thickness of 5-8 microns；The raw material group of the nano inorganic film Part and weight proportion are as follows: 8-10 parts of silica, 5-8 parts of magnesia, stabilized with yttrium oxide 15-20 parts of zirconium oxide, titanium carbide 5- 15 parts, 1-4 parts of carbon fiber, 8-10 parts of aluminium oxide, 5-8 parts of magnesium nitride, 3-4 parts of silicon nitride, 5-10 parts of silicon carbide, rice hull ash 15- 20 parts.

In the application, in plant extracts preparation process, used relevant device has, and the device of extraction includes heat pump Unit；The hot water apparatus of its water-cooling device and heat exchange with Cooling capacity exchanging；Condenser；It is with refrigerant first entrance Pipe, refrigerant first outlet pipe, the first water inlet pipe and the first outlet pipe for connecting water-cooling device；Coolant storage tank；It has connection cold The refrigerant second entrance pipe of matchmaker's first outlet pipe, the refrigerant second outlet pipe for being formed in coolant storage tank lower part, connection water-cooling device The second water inlet pipe and the second outlet pipe；Reactor tank；Its lower section for being set to coolant storage tank, the reactor tank have docking refrigerant the The refrigerant third inlet tube of two outlets, the third inlet tube are connected at the shower portion in reactor tank；The reactor tank Lower section is equipped with refrigerant third outlet；Discharge tank；Its 4th inlet tube of refrigerant, discharge tank for being equipped with connection refrigerant third outlet The first hot water inlet pipe and the first hot water outlet pipe that side is equipped with the 4th outlet of refrigerant, connects hot water apparatus；Thermal jacket pipe； It has connection the 4th outlet of refrigerant the 5th inlet tube of refrigerant, connect refrigerant first entrance pipe the 5th outlet of refrigerant, Connect the second hot water inlet pipe and the second hot water outlet pipe of hot water apparatus；The coolant storage tank, reactor tank and discharge tank it is outer Wrap up thermal insulation material in surface；The discharge tank is equipped with manual ball valve, docks essential oil recycling can below；The reactor tank has The lid that can be repeatedly opened or be closed；The condenser, coolant storage tank, reactor tank and discharge tank outer surface be equipped with water route Circulate the water tank to exchange heat；First water inlet pipe and the first outlet pipe are set on the water tank of condenser；Second water inlet Pipe and the second outlet pipe are set on the water tank of coolant storage tank；First hot water inlet pipe and the first hot water outlet pipe set out material On the water tank of tank；Second hot water inlet pipe and the second hot water outlet pipe set on the water tank of thermal jacket pipe.

Herbal extraction equipment used herein can also be high pressure mixing tank, and extraction material is placed in the high pressure mixing tank Material, high pressure mixing tank top are connected to high-pressure pump, and the lower part of high pressure mixing tank is connected to semipermeable membrane device one end, the semi-permeable membrane The other end of device is connected to intermediate air accumulator by check valve, and the intermediate air accumulator bottom end is connected to the defeated of condenser by valve Enter end, the output end connection extract liquor of the condenser collects ball, and the extract liquor collects ball and is also connected to activity carbon collecting device. The active carbon collection device is detachable installation.The feeding port of the high pressure mixing tank uses high pressure washer sealing.The extraction It takes liquid to collect ball to be made of transparent glass material.The condenser uses recirculated water heat exchange condensers.The microwave of plant extract Pass through valve with the gas outlet of supercritical CO 2 combined system, including carbon dioxide compression gas tank, the carbon dioxide compression gas tank Connection condenser, the condenser connection force (forcing) pump, the force (forcing) pump export connection heat exchanger, and heat exchanger passes through valve and extraction The bottom connection of tank, at the top of the extractor by valve with separate tower bottom connection, be equipped in the extractor and react sieve plate, It reacts and is equipped with microwave generating apparatus around sieve plate.The separation column is equipped with recovery channel, and the recovery channel passes through air pump Gas tank connection occurs with carbon dioxide.The knockout tower is the second-order separation tower, and the bottom of the knockout tower passes through valve and liquid out Pipe connection.

In the application, the preparation of rice hull ash used；

Step (1) removes it firstly, by the rice husk wash clean bought from Zhangjiakou City Wanquan County rice husk processing factory, drying In impurity, in case rice hull ash production use；

Temperature increasing schedule is arranged in step (2), and the firing maximum temperature of rice hull ash is set to 600 DEG C；Calcining system design are as follows: room Temperature is to 300 DEG C of heating 30min；300-400 DEG C of heating 20min；400-600 DEG C of heating 30min；600 DEG C of constant temperature 30min；600 DEG C-room temperature, Temperature fall；

1. 20 DEG C or so to 300 DEG C heating 30min；

2. 300-400 DEG C of heating 30min；

3. 400-600 DEG C of heating 30min；

4. 600 DEG C of constant temperature 30min；

5. 600-300 DEG C of cooling about 4h；

6. 300 DEG C to room temperature cool down about 1.5h.

The rice husk of drying is put into fire-clay crucible by step (3), and crucible is put into heating furnace and carries out burning processing；

Crucible taking-up is put into and is quickly cooled down outside window until descent of temperature is to after 300 DEG C or less by step (4), cold to temperature But manufactured rice hull ash is taken out from crucible afterwards, measuring and firing the main component of successful rice hull ash is SiO₂；

Step (5), the grinding of rice hull ash；(YJ-300 type high speed Universal pulverizer is good for the limited public affairs of Medical Devices by Jinan hundred million Department's manufacture, voltage rating 220V, power 1400W, 28000 revs/min of motor speed, powder fineness is 50-300 mesh) it will be after burning Rice hull ash is put into progress grinding processing in pulverizer, wherein rice hull ash makees the grinding processing of 2min, 3min, 4min；

Grinding rice hull ash is carried out XRD diffraction analysis with Antai Science and Technology Co., Ltd's X-ray diffractometer by step (6)；

Step 2, respectively every group weigh corresponding raw material；

Raw material by needed for each group is poured on mix plate progress mix 1min respectively by step 3, forms mixture

The mixing water for determining amount is poured into mixture stirring 2min by step 4

Step 5, casting；

Step 6, demoulding, are dried, 30-40 DEG C in an oven, dry 10-15h；

Step 7, sintering are sintered 5-7h at 900-1000 DEG C；

Step 8 obtains final products.

The material composition of rice husk are as follows: crude fibre 35.5%-45%, lignin 21%-26%, polycondensation pentose 16%-22%, Ash content 11.4%-22%, silica 1 0%-21% (being shown in Table 1).

The material composition of 1 rice husk of table

Essential element group becomes C, H, O, Si and also presss from both sides by a small amount of impurity in rice husk, this is just rice husk manufacture high-performance fertilizer And composite soil obtains extremely beneficial condition.And rice is as world-class crops, the annual output of paddy has been in recent years Reach more than 600,000,000 tons, and the China as large agricultural country, the annual output of rice also reach the half in modern times circle；And rice husk is as water The byproduct of rice, its yield is huge, is the 20% of paddy weight.But while there are many potential agricultural use, rice for rice husk The major part of shell has not found the method reasonably recycled.

The chemical component (%) of 2 rice hull ash of table

Detailed description of the invention

Fig. 1: the SEM figure of the application bioceramic film；

A kind of Fig. 2: microwave and supercritical CO extracted for plants essential oil of the present invention₂The structural schematic diagram of combined system；

Fig. 3 is the infrared spectrogram for the Semen Persicae extract that 1 method according to embodiments of the present invention obtains.

Fig. 4 is the wavelength scan curve figure of oleanolic acid of the invention.

Fig. 5 is the canonical plotting of oleanolic acid of the invention.

Fig. 6 is the curve graph of extraction temperature of the invention to Radix Angelicae Sinensis total saposins extraction rate impact.

Fig. 7 is the curve graph of extraction time of the invention to Radix Angelicae Sinensis total saposins extraction rate impact.

Fig. 8 is the curve graph of ethyl alcohol temperature of the invention to Radix Angelicae Sinensis total saposins extraction rate impact.

Fig. 9 is the curve graph of solid-liquid ratio of the invention to Radix Angelicae Sinensis total saposins extraction rate impact.

Figure 10 is the curve graph of pH of the invention to Radix Angelicae Sinensis total saposins extraction rate impact.

In figure, 1. carbon dioxide compression gas tanks, 2. extractors, 3. knockout towers, 4. condensers, 5. force (forcing) pumps, 6. microwaves hair Generating apparatus, 7. reaction sieve plates, 8. heat exchangers, 9. air pumps, 10. outlet tubes.

Beneficial effect

1, it is applicant's understanding that emphasis discloses the preparation work of plant extracts used herein in technical scheme Skill.Plant extract raw material used herein has a large amount of plant essence.The applicant is paid a large amount of by largely testing Creative labor, obtain the extraction process of plant extracts described herein and pass through the technique, the application one side energy Enough beneficial essences adequately extracted in plant, and this extract is used in combination with other components of capsule, it improves The effective component of Total saponin, Chrysophanol, amino acid in capsule, on the other hand, in gained capsule have Total saponin, Chrysophanol, The beneficial elements such as amino acid, this be in existing capsule technique field it is no, realize technological break-through, also sufficiently demonstrate Key and present invention point one of of the plant extracts preparation process in technical scheme.Through detecting, By the method for herein described plant extracts, extracted effective component Total saponin, Chrysophanol, amino acid compare conventional method 10% or so can be effectively improved by extracting the plant extracts yield, and purity can be improved 15-20%.

2, the application thinks: exactly these specific steps introduce, to obtain the capsule for having the characteristics that as described herein Object is laid a good foundation.

3, alcohol extracting is carried out to Radix Angelicae Sinensis in prescription, the influence factor that Radix Angelicae Sinensis total saposins extract is analyzed one by one, using orthogonal test Design optimizes the extracting method of Radix Angelicae Sinensis, improves the bioavilability of Radix Angelicae Sinensis.One of present invention is that Chinese angelica blood supplementing is living Blood improves body immunity, protection cardiovascular and cerebrovascular, diminishes inflammation and other effects, and effective component oleanolic acid has anti-well The physiological activity such as inflammation, antibacterial.Active constituent saponins water mentions that effect is bad, and effective component extraction efficiency and availability are not in Radix Angelicae Sinensis Greatly, therefore this patent carries out Radix Angelicae Sinensis to study independent extraction, improves its extraction efficiency and availability.

Specific embodiment

Embodiment 1

A kind of aloe cassia seed capsule of energy relaxing bowels to lose weight, the material component and its weight proportion of the capsule are as follows: plant 50 parts of extract, 10 parts of aloe powder, 15 parts of dietary fiber, 3 parts of thickener, 8 parts of gelatin, 3 parts of plasticizer, 30 parts of pure water.

The material component and weight of the plant extracts are as follows: 5 parts of Semen Persicae extract, 8 parts of cassia seed extract, 10 parts of angelica extract.

Embodiment 2

The material component and its weight proportion of the capsule are as follows: 70 parts of plant extracts, 20 parts of aloe powder, dietary fiber 25 Part, 8 parts of thickener, 13 parts of gelatin, 5 parts of plasticizer, 40 parts of pure water.

The material component and weight of the plant extracts are as follows: 10 parts of Semen Persicae extract, cassia seed extract 15 Part, 18 parts of angelica extract.

Embodiment 3

The material component and its weight proportion of the capsule are as follows: 75 parts of plant extracts, 21 parts of aloe powder, dietary fiber 26 Part, 9 parts of thickener, 24 parts of gelatin, 6 parts of plasticizer, 41 parts of pure water.

The material component and weight of the plant extracts are as follows: 8 parts of Semen Persicae extract, cassia seed extract 10 Part, 15 parts of angelica extract.

Total saponin experiment detection

1.1 laboratory apparatus and experimental material

1.1.1 laboratory apparatus

TU-1901 dual-beam ultraviolet specrophotometer (Beijing Puxi General Instrument Co., Ltd)；FZ-102 type is micro- Type plant pulverizer (Tianjin Stettlen instrument Co., Ltd)；RE-52AA Rotary Evaporators (the sub- flourish biochemical instrument in Shanghai Factory)；SB-5200DTD supersonic wave cleaning machine (Ningbo Xin Zhi biotechnology company limited by shares)；TP-214 electronic balance (Instrument Ltd., Denver).

1.1.2 experimental material Radix Angelicae Sinensis, lot number 20110425, is purchased from Anhui Jiren Pharmacy Co., Ltd..Olive acidity scale Quasi- product lot number is 110709-201005, is purchased from National Institute for Food and Drugs Control；Perchloric acid solution concentration is 0.1mol/L (self-control)；The ethyl alcohol that volume fraction is 95%；Remaining reagent is that analysis is pure.

1.2 experimental methods and result

1.2.1 the measuring method of Radix Angelicae Sinensis total saponin content

1.2.1.1 the preparation precision of reference substance solution weighs oleanolic acid standard items 11.0000mg, sets 50ml volumetric flask In, it is dissolved with dehydrated alcohol and is settled to scale.

1.2.1.2 the preparation of sample solution weighs a certain amount of dry angelica powder in a round bottom flask, adds in the ratio of 1:10 Enter ether (i.e. ether 10mL need to be added in angelica powder 1g), heating water bath flows back degreasing twice, and each 2h, temperature is controlled at 40 DEG C ~50 DEG C.It filters, the angelica powder after degreasing is dried for standby.

Precision weighs the angelica powder after 1.0007g degreasing, is 1:20 by solid-liquid ratio, that is, the second that volume fraction is 60% is added Alcohol 20mL is extracted twice, each 2h in 60 DEG C of water-baths.Combined extract, suction filtration, filtrate is after 0~5 DEG C of refrigeration for 24 hours, vacuum It is concentrated into paste.25mL water is added to redissolve, filters, the butanol solution extraction of filtrate water saturation, each 25mL is extracted repeatedly To n-butanol layer in until colourless, merge n-butanol layer, be washed with a small amount 2 times, be concentrated in vacuo to dry, is dissolved with dehydrated alcohol And it is settled to 100mL.

1.2.1.3 the determination of Detection wavelength is drawn 0.2mL oleanolic acid standard solution and sample solution respectively and is filled in tool In test tube, 70 DEG C of water-baths volatilize solvent.5% vanillic aldehyde-glacial acetic acid solution the 0.2mL newly prepared is added, adds 0.8mL high Solution chlorate heats 15min in 70 DEG C of water-baths, takes out, and the cooling 10min of flowing water is allowed to fully reacting.4mL acetic acid second is added Ester shakes up.To accompany, reagent makees blank, is scanned in 450~600nm wave-length coverage, determines maximum absorption wavelength.As a result See Fig. 4.

As a result: as can be seen from Figure 4, oleanolic acid standard solution has maximum absorption band at 545nm, and sample has stronger suction It receives.Therefore select 545nm as measurement wavelength.

1.2.1.4 the foundation precision of the drafting of standard curve and regression equation draws oleanolic acid standard solution 0mL, 1mL, 2mL, 5mL, 8mL, 10mL are diluted to scale in 10ml volumetric flask, with dehydrated alcohol, by " 1.2.1.3 Detection wavelength Method under determination " item, measures absorbance at 545nm, and using absorbance as ordinate, the concentration of oleanolic acid is abscissa, draws Standard curve processed, is shown in Fig. 5.

As a result: regression equation: correlation coefficient r=0.9993 Y=0.0074X+0.0146, equation is in 0~220 μ g/ml model There is good linear relationship in enclosing.

1.2.1.5 the measurement precision of total saponin content draws 0.2mL oleanolic acid sample solution in tool plug test tube, presses 1.2.1.3 the method under item surveys absorbance at 545nm, is according to total saposins concentration in regression equation calculation sample solution 200.2 μ g/mL, are calculated as follows its recovery rate.

Recovery rate:In formula: C is total saposins concentration (μ g/mL)；V is the total volume of extracting solution (mL)；W is the quality (g) of degreasing angelica powder used.

1.2.2 methodology is examined or check

1.2.2.1 stability experiment precision draws 0.2mL oleanolic acid sample solution, surveys an absorbance every 10min, It calculates RSD (the results are shown in Table 3).

Table 3: stability experiment

Serial number	Time/min	Absorbance A
			1	10	0.382
2	20	0.387
			3	30	0.384
4	40	0.391
			5	50	0.392
6	60	0.393

As a result: the absorbance change of sample is little in lh, basicly stable, RSD=1.16%.Show the sample stability Well.

1.2.2.2 Precision Experiment precision draws 0.2mL oleanolic acid standard solution, totally 5 parts, surveys absorbance, calculates RSD value (the results are shown in Table 4).

Table 4: Precision Experiment

Serial number	Absorbance A
		1	0.376
2	0.371
		3	0.379
4	0.367
		5	0.379

As a result: calculating RSD=1.41%, show that the precision of this method is good.

1.2.2.3 sample recovery rate experiment draws 5 parts of 0.1~0.5mL sample solution, respectively plus people 0.1mL (22.0 μ g) Oleanolic acid standard solution surveys absorbance, calculates concentration, and the rate of recovery and RSD value (the results are shown in Table 5) is calculated as follows.

Table 5: sample recovery rate experiment

Test serial number	Sample/μ g	Standard items/μ g	Measured value/ug	Sample recovery rate/% (wt)
					1	20.01	22.0	42.26	100.6
2	40.02	22.0	61.71	99.5
					3	60.03	22.0	82.35	100.4
4	80.04	22.0	101.47	99.4
					5	100.05	22.0	124.65	102.1

As a result: calculating average recovery rate is 100.4% (wt), and the measurement result of RSD=1.2%, this method are reliable.

1.2.3 the Study on extraction of Radix Angelicae Sinensis total saposins influences having for saponin extraction principal element: temperature, time, ethyl alcohol Concentration, solid-liquid ratio, pH value etc..To study influence of each factor to total saposins recovery rate, single factor experiment and orthogonal examination are carried out It tests.

1.2.3.1 influence of the temperature to recovery rate accurately weighs 5 parts of 1.001g Radix Angelicae Sinensis coarse powder, by solid-liquid ratio 1:20 (g:mL) Addition volume fraction is 60% ethyl alcohol, that is, addition volume fraction is 60% ethyl alcohol 20mL, respectively in 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, extract 90min at 80 DEG C, Fig. 6 is shown in influence of the temperature to the recovery rate of total saposins.Fig. 6 is extraction temperature of the invention to wood The curve graph of melon total saposins extraction rate impact.

As a result: from fig. 6, it can be seen that as the temperature rises, the recovery rate of saponin(e is gradually increased, reaching most at 70 DEG C Greatly, temperature is continued growing, the recovery rate of saponin(e is declined, therefore optimum extraction temperature is 70 DEG C.

1.2.3.2 influence of the extraction time to recovery rate accurately weighs 5 parts of 1.003g Radix Angelicae Sinensis coarse powder, by solid-liquid ratio 1:20 (g:mL) it is 70% ethyl alcohol that volume fraction, which is added, i.e. addition volume fraction is 70% ethyl alcohol 20mL, is extracted respectively at 70 DEG C 30min, 60min, 90min, 120min and 150min.Fig. 7 is shown in influence of the extraction time to the recovery rate of total saposins.As a result: from Fig. 7 can be seen that with the extension of time, the recovery rate of total saposins is continuously increased, and when 120min reaches maximum, later total saposins Recovery rate ease up slow decline, the optimum extraction time is 120min.

1.2.3.3 influence of the concentration of alcohol to recovery rate accurately weighs 5 parts of 0.999g Radix Angelicae Sinensis coarse powder, is separately added into volume point The ethyl alcohol 20mL that number is 30%, 45%, 60%, 75% and 90%, extracts 120min, concentration of alcohol is to total soap respectively at 70 DEG C Fig. 8 is shown in the influence of the recovery rate of glycosides.

As a result: from figure 8, it is seen that the recovery rate of saponin(e is also increasing, and concentration of alcohol reaches with the increase of concentration of alcohol Leaching rate is maximum when to 75% (volume fraction), but concentration continues to increase the recovery rate of saponin(e and can decline instead, this mainly with work as Return the polarity of saponin(e related, according to the similar principle that mixes, preferably selecting volume fraction for 75% ethyl alcohol is optimum extraction agent concentration.

1.2.3.4 influence of the solid-liquid ratio to recovery rate accurately weighs 5 parts of about 1.001g Radix Angelicae Sinensis coarse powder, presses solid-liquid ratio l respectively: The ethyl alcohol that volume fraction is 75% is added in 10 (g:mL), l:15 (g:mL), l:20 (g:mL), 1:25 (g:mL), 1:30 (g:mL), It is separately added into ethyl alcohol 10mL, 15mL, 20mL, 25mL, 30mL that volume fraction is 75%, is extracted respectively at 70 DEG C Fig. 9 is shown in 120min, influence of the solid-liquid ratio to the recovery rate of total saposins.

As a result: from fig. 9, it can be seen that with the increase of solid-liquid ratio, the recovery rate of saponin(e be increased, but increased amplitude Less.Solid-liquid ratio is excessive, and consumption solvent is more, in concentration technology also can more time consumption and energy consumption, therefore best solid-liquid ratio 1:20 (g:mL).

1.2.3.5 influence of the pH to recovery rate accurately weighs 5 parts of about 1.002g Radix Angelicae Sinensis coarse powder, by solid-liquid ratio 1:20 (g: ML) be added volume fraction be 75% ethyl alcohol, i.e., addition volume fraction be 75% ethyl alcohol 20mL, respectively adjust pH be 3,5,7, 9,11 extraction 120min.Figure 10 is shown in influence of the pH to the recovery rate of total saposins.

As a result: it is very big that Figure 10 can be seen that influence of the pH to saponin extraction rate, when pH=7, saponin extraction rate highest.

1.2.3.6 optimization of orthogonal test technological parameter is the influence degree and reciprocation for investigating each factor, selection pair Four factors that saponin extraction is affected, each factor select three levels, carry out L₉(3⁴) orthogonal test.Factor level is shown in Table 6, orthogonal experiments are shown in Table 7.

Table 6: factor level table

It is horizontal	A(/℃)	B(/min)	C (/ %)	D(pH)
					1	60	60	60	6
2	70	90	75	7
					3	80	120	90	8

Table 7: orthogonal experiments

As a result: influence degree being extracted to Radix Angelicae Sinensis total saposins are as follows: C > D > A > B, i.e. concentration of alcohol > pH > temperature > time.Most preferably Extraction conditions are as follows: C₂D₂A₂B₃, i.e., temperature 70 C, time 120min, concentration of alcohol are 75% (volume fraction), pH=7.

1.3 conclusion

The present invention is first extracted with ether by angelica powder degreasing, then with n-butanol repeatedly, thus reduce in Radix Angelicae Sinensis it is other at The interference divided.Colorimetric analysis has been carried out with ultraviolet spectrophotometry, since colorimetric method is for substance similar in structure, has been developed the color sensitive Degree is high, easy to operate, and reproducibility is preferable, therefore is suitable for the assay of total saposins.

Finally, it should be noted that obviously, above-described embodiment is only intended to clearly illustrate the application example, and simultaneously The non-restriction to embodiment.For those of ordinary skill in the art, it can also do on the basis of the above description Other various forms of variations or variation out.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn Shen go out obvious changes or variations still in the protection scope of the application type among.

Claims (5)

1. a kind of aloe cassia seed capsule of energy relaxing bowels to lose weight, which is characterized in that the material component and its weight of the capsule are matched Than are as follows: 50-70 parts of plant extracts, 10-20 parts of aloe powder, 15-25 parts of dietary fiber, 3-8 parts of thickener, 8-13 parts of gelatin, 3-5 parts of plasticizer, 30-40 parts of pure water.

2. a kind of aloe cassia seed capsule of energy relaxing bowels to lose weight according to claim 1, which is characterized in that the capsule Material component and its weight proportion are as follows: 50 parts of plant extracts, 10 parts of aloe powder, 15 parts of dietary fiber, 3 parts of thickener, gelatin 8 Part, 3 parts of plasticizer, 30 parts of pure water.

3. a kind of aloe cassia seed capsule of energy relaxing bowels to lose weight according to claim 1, which is characterized in that the capsule Material component and its weight proportion are as follows: 70 parts of plant extracts, 20 parts of aloe powder, 25 parts of dietary fiber, 8 parts of thickener, gelatin 13 parts, 5 parts of plasticizer, 40 parts of pure water.

4. a kind of aloe cassia seed capsule of energy relaxing bowels to lose weight according to claim 1, which is characterized in that the plant mentions Take the material component and weight of object are as follows: 5-10 parts of Semen Persicae extract, 8-15 parts of cassia seed extract, angelica extract 10-18 parts.

5. the preparation method of aloe cassia seed capsule described in a kind of claim 1, which is characterized in that the method includes walking as follows It is rapid:

Step 1: raw material preparation；

Step 2: crushing；

Step 3: dry；

Step 4: sieving；

Step 5: mixing；

Step 6: dress capsule；

Step 7: packaging；

Step 8: irradiation sterilization.