CN103919890A - Preparation method of effervescent tablet of pericarp and pomace extract of citrus Changshan-huyou - Google Patents
Preparation method of effervescent tablet of pericarp and pomace extract of citrus Changshan-huyou Download PDFInfo
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Abstract
The invention relates to a preparation method of an effervescent tablet of a pericarp and pomace extract of citrus Changshan-huyou, belonging to the technical field of preparation methods of plant active components. The preparation method comprises the following technical steps: 1) weighing raw materials; 2) pelletizing separately by acid and base; 3) pelletizing by acid and base and drying, mixing, grinding and tabletting to obtain the effervescent tablet of the pericarp and pomace extract of citrus Changshan-huyou. According to the preparation method provided by the invention, by taking fruit dregs of citrus Changshan-huyou as the raw materials, an effective component extraction technology is established to extract limonin and flavonoid substances so as to develop and research the effervescent tablet with the function of reducing blood fat, thereby satisfying the current blood fat-reducing health-care product market. The effervescent tablet has a wide market prospect. Meanwhile, deep processing of fruit industry and utilization of processing byproducts are promoted, the economical benefit is improved, and the environmental pollution is reduced, so that the preparation method provided by the invention has important actual guiding significance.
Description
Technical field
The invention belongs to the preparation method technical field of active components of plants, be specifically related to the preparation method of the effervescent tablet of Changshan grapefruit peel marc extract.
Background technology
Changshan grapefruit has another name called golden Fructus Citri grandis, is a novel species of China's orange of being formed by Fructus Citri grandis and orange natural hybrization, originates in Changshan County, Zhejiang Province, existing over one hundred year so far cultivation history.Because of its fruit good looking appearance, suitable size, color and luster is tempting, fragrance is unique, mouthfeel is fresh and crisp, and nutritious, utmost point storage tolerance, thereby the favor of Shen Shou consumer, it is a kind of desirable fruit of eating raw, also be that one well processes raw material, economic worth is very high, and repeatedly prize-winning in the comparation and assessment of the whole nation, become the assorted Citrus chachiensis Hort. of first high-quality of China, be known as " the assorted Citrus chachiensis Hort. of China first ".
According to statistics, 130,000 tons of Zhejiang Province's Changshan grapefruit annual productions, but due to reasons such as fruit qualities, the economic benefit of Changshan grapefruit increases progressively slowly, even occurs the phenomenon of some areas excess production capacity, and the skin slag garbage of Changshan grapefruit has caused certain environmental pollution simultaneously.Therefore, deep processing technology, the especially comprehensive utilization to fruit skin slag garbage of research Changshan grapefruit, be to improve industrial benefit, the important channel of reducing skin slag waste pollution.
Summary of the invention
The problem existing for prior art, the object of the invention is to design provides a kind of technical scheme of preparation method of effervescent tablet of Changshan grapefruit peel marc extract.
The preparation method of the effervescent tablet of described Changshan grapefruit peel marc extract, is characterized in that comprising following processing step:
1) take each raw material according to following weight proportion
Changshan grapefruit peel marc extract powder 5～15%, citric acid and sodium carbonate 40～50%, dextrin 30～50%, dehydrated alcohol 2～8%, PEG-4000 0.2～1%, described citric acid: the weight ratio of sodium carbonate is 1.6:1;
2) get above-mentioned each raw material and cross 80 mesh sieves, Changshan grapefruit peel marc extract powder is evenly divided into two parts to be mixed with citric acid and sodium carbonate respectively, in Acid-Base System, add respectively dextrin to do filler, using dehydrated alcohol as binding agent, 24 orders are granulated and are carried out separately granulation of soda acid;
3) soda acid granulation being put into 40～70 DEG C of thermostatic drying chambers is dried; after being dried; soda acid is granulated and mixed; add the PEG-4000 of described weight proportion; grind; after it is fully mixed, under pressure 3～10Mpa, carry out tabletting, obtain the effervescent tablet of Changshan grapefruit peel marc extract.
The preparation method of the effervescent tablet of described Changshan grapefruit peel marc extract, is characterized in that described Changshan grapefruit peel marc extract powder makes by following steps:
A) get fresh Changshan grapefruit peel marc shred successively, 60 DEG C dry and pulverization process, obtain powder;
B) get the powder 95% alcoholic solution reflux that step 1) obtains and carry out three extractings, 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, obtain oil-like extracts;
C) get step 2) oil-like extracts that obtains adds petroleum ether to carry out ungrease treatment, and oil-like extracts and petroleum ether by volume 1:1 mix and extract, and take off a layer extract volatilization petroleum ether and obtain extract after defat after extraction;
D) after extracting degreasing, extract utilizes D101 type macroporous resin to carry out column chromatography, with the ethanol elution of concentration 20～80%, collects eluent, and eluent revolves steaming, pulverizes to obtain Changshan grapefruit peel marc extract powder.
The preparation method of the effervescent tablet of described Changshan grapefruit peel marc extract, is characterized in that taking each raw material by Changshan grapefruit peel marc extract powder 7～12%, citric acid and sodium carbonate 42～48%, dextrin 35～45%, dehydrated alcohol 3～6% and PEG-4000 0.4～0.8% in described step 1).
The preparation method of the effervescent tablet of described Changshan grapefruit peel marc extract, is characterized in that taking each raw material by Changshan grapefruit peel marc extract powder 10%, citric acid and sodium carbonate 45%, DEXTRIN %, dehydrated alcohol 4.5%, PEG-4000 0.5% in described step 1).
The preparation method of the effervescent tablet of described Changshan grapefruit peel marc extract, is characterized in that in described step 3), thermostatic drying chamber bake out temperature is 40 DEG C.
The preparation method of the effervescent tablet of described Changshan grapefruit peel marc extract, is characterized in that described step 3) tabletting pressure is 6Mpa.
The present invention, taking Changshan grapefruit fruit skin slag garbage as material, sets up extracts active ingredients technology, extracts limonin and Flavonoid substances, and research and development have the effervescent tablet of hypolipemic function, meet current blood fat reducing health products market, have wide market prospect.Promote the utilization of fruit industry deep processing and processing byproduct simultaneously, increase economic efficiency, reduce environmental pollution, there is important actual directive significance.
Brief description of the drawings
Fig. 1 Flavonoid substances canonical plotting;
Fig. 2 limonin substances canonical plotting.
Detailed description of the invention
Further illustrate the present invention below in conjunction with embodiment.
Embodiment 1: the preparation of mountain grapefruit peel marc extract
1) get that fresh Changshan grapefruit peel marc shreds successively, 60 DEG C of oven for drying and pulverization process, obtain powder;
2) get the powder 95% alcoholic solution reflux that step 1) obtains and divide three extractings, 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, obtain oil-like extracts;
3) get step 2) oil-like extracts that obtains and petroleum ether mix and extract by 1:1 by volume, repeats 5 times, takes off a layer extract volatilization petroleum ether after extraction, obtains extract after defat;
4) after extracting degreasing, extract utilizes D101 type macroporous resin to carry out column chromatography, with the ethanol elution eluting of concentration 20～80%, collects eluent, and eluent revolves steaming, pulverizes to obtain Changshan grapefruit peel marc extract powder.
Embodiment 2: the preparation of mountain grapefruit peel marc extract effervescent tablet
Changshan grapefruit peel marc extract powder and each adjuvant that embodiment 1 is obtained, that is: citric acid, sodium carbonate, dextrin, each mistake 80 mesh sieves of PEG-4000; Changshan grapefruit peel marc extract powder is divided into two parts to be mixed with citric acid and sodium carbonate respectively, in Acid-Base System, add respectively dextrin to do filler, using dehydrated alcohol as binding agent, 24 orders are granulated and are carried out separately granulation of soda acid, wherein acid source is mixed by Changshan grapefruit peel marc extract powder 5%, sodium carbonate 17.3%, dextrin 20%, using dehydrated alcohol 2.25% as binding agent, 24 orders are granulated and are obtained; Alkali source is mixed by Changshan grapefruit peel marc extract powder 5%, citric acid 27.7%, dextrin 20%, and using dehydrated alcohol 2.25% as binding agent, 24 orders are granulated and obtained; Soda acid granulation is put into 40 DEG C of thermostatic drying chambers and be dried, after being dried, soda acid is granulated and mixed; add PEG-4000 0.5%, grind, after it is fully mixed; under pressure 6Mpa, carry out tabletting, obtain the effervescent tablet of Changshan grapefruit peel marc extract.
Embodiment 3: the preparation of mountain grapefruit peel marc extract effervescent tablet
Changshan grapefruit peel marc extract powder and each adjuvant that embodiment 1 is obtained, that is: citric acid, sodium carbonate, dextrin, each mistake 80 mesh sieves of PEG-4000; Changshan grapefruit peel marc extract powder is divided into two parts to be mixed with citric acid and sodium carbonate respectively, in Acid-Base System, add respectively dextrin to do filler, using dehydrated alcohol as binding agent, 24 orders are granulated and are carried out separately granulation of soda acid, wherein acid source is mixed by Changshan grapefruit peel marc extract powder 6%, sodium carbonate 18.5%, dextrin 17.5%, using dehydrated alcohol 2.1% as binding agent, 24 orders are granulated and are obtained; Alkali source is mixed by Changshan grapefruit peel marc extract powder 6%, citric acid 29.5%, dextrin 17.5%, and using dehydrated alcohol 2.1% as binding agent, 24 orders are granulated and obtained; Soda acid granulation is put into 50 DEG C of thermostatic drying chambers and be dried, after being dried, soda acid is granulated and mixed; add PEG-4000 0.8%, grind, after it is fully mixed; under pressure 3Mpa, carry out tabletting, obtain the effervescent tablet of Changshan grapefruit peel marc extract.
Embodiment 4: the preparation of mountain grapefruit peel marc extract effervescent tablet
Changshan grapefruit peel marc extract powder and each adjuvant that embodiment 1 is obtained, that is: citric acid, sodium carbonate, dextrin, each mistake 80 mesh sieves of PEG-4000; Changshan grapefruit peel marc extract powder is divided into two parts to be mixed with citric acid and sodium carbonate respectively, in Acid-Base System, add respectively dextrin to do filler, using dehydrated alcohol as binding agent, 24 orders are granulated and are carried out separately granulation of soda acid, wherein acid source is mixed by Changshan grapefruit peel marc extract powder 3.5%, sodium carbonate 16.2%, dextrin 22.5%, using dehydrated alcohol 2.8% as binding agent, 24 orders are granulated and are obtained; Alkali source is mixed by Changshan grapefruit peel marc extract powder 3.5%, citric acid 25.8%, dextrin 22.5%, and using dehydrated alcohol 2.8% as binding agent, 24 orders are granulated and obtained; Soda acid granulation is put into 70 DEG C of thermostatic drying chambers and be dried, after being dried, soda acid is granulated and mixed; add PEG-4000 0.4%, grind, after it is fully mixed; under pressure 10Mpa, carry out tabletting, obtain the effervescent tablet of Changshan grapefruit peel marc extract.
Embodiment 5: in Changshan grapefruit peel marc extract, the mensuration of Flavonoid substances and limonin substances and optimised process determines
1 materials and methods
1.1 experiment materials, instrument, reagent and reagent
1.1.1 experiment material
Changshan grapefruit (being purchased from local fruit market, Changshan County, Zhejiang Province)
1.1.2 key instrument
GZX-9140 MBE digital display air dry oven (Shanghai Medical Equipment Plant of Bo Xun Industrial Co., Ltd.), UV-1800 ultraviolet-uisible spectrophotometer (SHIMADZU CORPORATION(Shimadzu)), PL-203 electronic balance (METTLER TOLEDO(prunus mume (sieb.) sieb.et zucc. Teller-Tuo benefit) instrument (Shanghai) Co., Ltd.), HWS26 thermostat water bath (Shanghai Yi Heng Science and Technology Ltd. Shanghai one permanent scientific and technological Instrument Ltd.), Sorvall ST 16R refrigerated centrifuger (Thermo Scientific), FiveEasy Plus pH meter (METTLER TOLEDO(prunus mume (sieb.) sieb.et zucc. Teller-Tuo benefit) instrument (Shanghai) Co., Ltd.), desk type powder tablet machine (Tianjin Si Chuanjingshi development in science and technology company limited)
1.1.3 reagent and reagent
Rutin (>=98%, be purchased from Jin Sui bio tech ltd, Shanghai), limonin (>=98%, be purchased from Jin Sui bio tech ltd, Shanghai), obaculactone (>=98%, be purchased from Aladdin reagent company), 4-Nitrophenyl butyrate (Lot#111M5207V is purchased from SIGMA reagent company of the U.S.), pancreatic lipase (Lot#SLBC9250V, be purchased from SIGMA reagent company of the U.S.), olive oil (chemical pure is purchased from Aladdin reagent company)
1.2 experimental technique
1.2.1 pretreatment of raw material
Get fresh Changshan grapefruit skin test sample, after shredding, put into 60 DEG C of baking ovens and dry, be ground into powder with cooking machine, obtain powder 1647g, for subsequent use.
1.2.2 Flavonoid substances and limonin substances extract purification
95% alcoholic solution reflux is carried out extracting, and point three extractions, 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, obtain oil-like extracts 500mL.Utilize D101 type macroporous resin to carry out column chromatography, use respectively 20%, 40%, 60%, 80%, 95% ethanol elution, extracting solution revolves and steams to obtain sample powder, is Flavonoid substances and limonin substances.
1.2.3 the content assaying method of functional components
1.2.3.1 Flavonoid substances assay
(1) preparation of rutin storing solution
Take 6.20mg control substance of Rutin in beaker with electronic balance, add 15ml ethanol solution, be placed in thermostat water bath and be heated to rutin and dissolve.Be transferred in the brown volumetric flask of 25ml, add dehydrated alcohol standardize solution; Take 0.6676g AlCl3 solid with electronic balance and be configured to 50mL AlCl3 solution.Collocation method: 36%-38% hydrochloric acid solution, by joining with the volume ratio of distilled water 1:3 the hydrochloric acid 40mL that is about 10% in beaker, slowly adds AlCl3 powder, stirs, until dissolve completely, is transferred in 50mL volumetric flask, then adds distilled water to be settled to 50mL; Take sodium acetate solid 0.8208g in beaker with electronic balance, be settled to 50mL with distilled water, add acetum and be adjusted to pH=5.2.
(2) preparation of rutin standard solution
Get respectively rutin storing solution 0.0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL, be placed in 25 mL volumetric flasks, add sodium acetate buffer solution 1 mL of AlCL3 solution 2 mL, the pH=5.2 of 0.1 mol/L, be settled to scale with dehydrated alcohol, shake up.After 40 DEG C of water-bath 10 min, taking-up volumetric flask is put into water and is cooled to room temperature.
(3) selection of mensuration wavelength
Measure respectively need testing solution, the each 1.0mL of rutin storing solution, be placed in respectively 25mL measuring bottle, respectively add the sodium acetate buffer solution 1.0mL of 0.1mol/L aluminum trichloride solution 2.0mL and pH=5.2, add 30% ethanol dilution to scale, shake up, 40 DEG C of water-bath 10 min.Obtain blank solution with legal system.By ultraviolet one visible spectrophotometry (annex VA of Pharmacopoeia of the People's Republic of China version in 2010) experiment, in the interscan of 200-500 nm wave-length coverage, record ultra-violet absorption spectrum, obtaining the suitableeest wavelength is 360nm.
(4) drafting of standard curve
The absorbance of measuring each concentration rutin titer at 360nm wavelength place, drawing standard curve, obtains regression equation.As shown in Figure 1.
(5) sample size is measured
Accurately take 20%, 40%, 60%, 80% the each 8.0mg of ethanol elution thing powder, add in beaker, add dehydrated alcohol 15mL, in thermostat water bath, slight fever is dissolved, and the temperature setting of thermostat water bath is set to 50 DEG C.After dissolving completely, take out, be cooled to room temperature, be transferred in the brown volumetric flask of 25mL, be diluted to scale with dehydrated alcohol, shake up.Respectively get 3.0mL in the brown volumetric flask of 25mL, and numbering is respectively 1,2,3,4.The sodium acetate buffer solution 1.0mL that adds 0.1 mol/L aluminum trichloride solution 2.0 mL and pH=5.2, adds dehydrated alcohol and is settled to scale, shakes up.40 DEG C of water-bath 10 min, take out.Simultaneously using dehydrated alcohol as blank.Measure light absorption value at 360nm place, by each concentration ethanol eluate sample light absorption value substitution regression equation, calculate Flavonoid substances content in each concentration ethanol eluate.
1.2.3.2 limonin substances assay
(1) preparation of developer
Accurately take 125.0mg two-methylamino phenenyl formaldehyde is dissolved in to 100.0mL sulphuric acid: in dehydrated alcohol (V sulphuric acid: V dehydrated alcohol=35:65) mixed liquor, add 0.5mL 0.9% liquor ferri trichloridi, now with the current.
(2) drafting of standard curve
Accurately take limonin standard substance 10.0mg, be placed in 20mL beaker, use a small amount of anhydrous alcohol solution, be transferred in 10mL volumetric flask, use dehydrated alcohol standardize solution, shake up, be made into the standard solution of 1mg/mL, for subsequent use.Separately get 5 10mL volumetric flasks, add respectively 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL standard solution, add respectively again developer 5.0mL, shake up, add dehydrated alcohol to be settled to scale, after leaving standstill 30min, measure absorbance in 500nm wavelength place, taking blank solution as reference, taking standard substance concentration as abscissa, absorbance is vertical coordinate, drawing standard curve, obtains regression equation.As shown in Figure 2.
(3) sample size is measured
Accurately pipette a certain amount of standard solution or sample solution in volumetric flask, add nitrite ion, shake up, leave standstill, make reference with blank reagent, survey its absorbance at specified wavelength place.Absorbance substitution regression equation, obtains the content of limonin.
1.2.3.3 effect for reducing fat determination of activity
Pancreatic lipase is the most important enzyme of hydrolysis dietary fat, the acidic protein molecule that isoelectric point, IP is 5.0.The food fat of hydrolyzable 50%-70%, can control hyperlipidemia by suppressing pancreatic lipase activity.Measure determinand and just can carry out effect for reducing fat evaluation to the inhibition activity of pancreatic lipase.
(1) experimental principle
Utilize pancreatic lipase that olive oil hydrolysis is generated to fatty acid and glycerol, copper ion reaction in fatty acid and developer generates Copoloid blue complex, under 710nm wavelength, there is obtained the maximum absorption, then contrast fatty acid absorbance working curve and draw the concentration of fatty acid, calculate the activity of enzyme.
(2) experimental implementation (Copoloid method is measured active)
The preparation of a reaction mixture (5.80mL substrate)
Mass concentration is 50g/L arabic gum: gets appropriate arabic gum, adds distilled water preparation, and standardize solution, for subsequent use.
Tris-HC1 buffer (20mol/L, pH=7.7): measure Tris2.4228g in beaker, add appropriate distilled water and dissolve, add HCl, utilize PH agent to regulate and make PH=7.7.Adding distil water is settled to 1000mL again.Getting appropriate mass concentration is that 50g/L arabic gum is dissolved in buffer.
Mass concentration is 50g/L Schweinfurt green solution (developer): Schweinfurt green solution pyridine is adjusted to pH=6.0.
The HCl solution of preparation 6mol/L: really measure 36%-38%HCl solution 51.1mL, thin up, is settled to 100mL.
Pancreatic lipase solution (5mg/mL, about 200U/mL): take 50mg pancreatic lipase, dissolve with appropriate Tris-HC1 buffer (75 mol/L, pH=7.4), the centrifugal 5min of 16000r/min, is settled to 1O mL with Tris-HC1 buffer.10mL is divided into after two parts, gets a copy of it and boil deactivation.Preparation before each use.
Olive oil substrate preparation: the 20mol/LTris-HCl buffer mixing of getting 0.5mL olive oil, 4.50mL normal hexane, 0.80mL makes.
Ethanol extraction solution: with dissolve with methanol, making ethanol extraction final mass concentration is 1000 μ g/mL, 800 μ g/mL, 600 μ g/mL, 400 μ g/mL, 200 μ g/mL, 100 μ g/mL, 50 μ g/mL, 25 μ g/mL and 12.5 μ g/mL.Every group establish 3 parallel.
Determining of b working sample group and matched group
Experiment arranges sample sets, blank group, positive controls, negative control group, gets a certain amount of Tris-HCl buffer, enzymatic solution and sample for each group, in table 1.After 37 DEG C of insulation 15min, add the HCl solution cessation reaction of the 6mol/L of 1mL.
Table 1 ethanol extraction is to lipase inhibition experiment (mL)
C chromogenic reaction
Draw supernatant 0.40mL in centrifuge tube, the mass concentration that adds 4.6mL toluene and 1.0mL is 50g/L Schweinfurt green solution (Schweinfurt green solution pyridine is adjusted pH to 6.0), centrifuge tube vortex 60 seconds.
D measures the selection of wavelength
Use UV-1800 spectrophotometer all band scanning toluene phase, find wavelength corresponding to peak value place.
The drafting of e oleic acid standard curve
Get respectively oleic acid 0.0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL, dilution standardize solution.Measure the light absorption value of each concentration rutin standard at the wavelength place of selecting.Drawing standard curve, obtains regression equation.
The determination of activity of f sample
Add after the copper reactant of 1.0mL in mutually toward toluene, the free fatty (FFAs) of toluene in mutually will be separated.The amount of free fatty is determined by the standard curve of oleic acid.Get the solution after appropriate chromogenic reaction, measure its absorbance at the wavelength place of selecting.Substitution standard curve can obtain fatty acid concentration.
G is active to be calculated
The active computing formula of enzyme is:
Lipase activity=CV/TV1
In formula, C represents the concentration of fatty acid, and V represents the volume (ml) of fatty acid-benzole soln, and T represents action time (min), and V1 represents enzyme liquid consumption (mL).
H ethanol extraction suppression ratio calculates
According to calculating gained lipase active, calculate suppression ratio.
Suppression ratio (%)=(matched group-experimental group)/matched group
1.3 health product (effervescent tablet) process optimization
1.3.1 extract ungrease treatment
After application of sample, first wash with water.Macroporous resin the macromolecular substances such as water soluble polysaccharide, phlegmatic temperament is not adsorbed or absorption affinity a little less than, water can be by its eccysis, can make extract obtain certain purification.
Ethanol extraction contains a large amount of volatile oil compositions, if directly use D101 macroporous resin eluting, more serious to the damage ratio of macroporous resin, and loading just needs regeneration for 3 times afterwards.Therefore, ethanol extraction first need be carried out to defat, the petroleum ether of same volume extracts, and repeats after 5 times, lower floor's extract is left standstill in fume hood to 30min, and guarantee petroleum ether is removed completely.
Get the grease 5mL of pretreatment gained in separatory funnel, the petroleum ether that adds same volume extracts, and repeats after 5 times, lower floor's extract is left standstill in fume hood to 30min, and guarantee petroleum ether is removed completely, even extract ungrease treatment.
1.3.2 the different proportion research of extract, citric acid and sodium carbonate
Consider citric acid and the total consumption of sodium carbonate, citric acid and the impact of sodium carbonate ratio on finished product in effervescent tablet, design this two factorial experimentss (table 2), investigate tabletting situation, change color and disintegration.
The different proportioning tests of table 2 adjuvant are probed into
1.3.3 the optimization of preparation condition
1.3.3.1 probe into the impact of baking temperature on finished product
In effervescent tablet production process, in granulating process, the difference of baking temperature used has a certain impact to its hydroscopicity.The granulation baking temperature of 40 DEG C, 50 DEG C, the 70 DEG C impact on effervescent tablet hydroscopicity is selected in this experiment.The soft material making is prepared to granule by following three kinds of techniques, and carry out the experiment of hydroscopicity mensuration.
Table 3 process optimization---probe into the impact of baking temperature on end product quality
1.3.3.2 the impact of different pressures on finished product
In effervescent tablet production process, in granulating process, disintegration time and the effervescent effect of the difference of the pressure of tablet machine used to effervescent tablet has a certain impact.A certain amount of effervescent tablet of the pressure system of 3Mpa, 6Mpa, 10Mpa is selected in this experiment, and evaluation to its effervescent effect of being correlated with.
1.3.3.3 different pressures and the impact of effervescent temperature on end product quality
In effervescent tablet production process, when film-making, the difference of pressure used has a certain impact to its tabletting situation.Simultaneously, in the time carrying out effervescent tablet disintegrate experiment, effervescent water temperature used also can be on producing certain impact disintegration, 3Mpa, 6Mpa, the 10Mpa pressure pressure as tabletting is selected in this experiment, design water temperature is 15 DEG C, 20 DEG C, 35 DEG C water temperatures during for effervescent, test, tabletting effect and effervescent effect to effervescent tablet are evaluated.
Table 4 process optimization-probe into tabletting pressure and the impact of effervescent temperature on end product quality
1.3.4 quality testing
Tablet should meet following pertinent regulations in production with duration of storage: the medicated powder (cream) for film-making is answered and mixed homogeneously with adjuvant.Content of dispersion little or containing the tablet of toxic medicine, should make dispersion of medicine by suitable method according to the character of medicine.
" Chinese Pharmacopoeia " clearly specifies, tablet must carry out weight differential, disintegration, limit test of microbe, to ensure the quality of tablet.
1.3.4.1 the mensuration of hydroscopicity
The glass exsiccator that bottom is filled to NaCl supersaturated aqueous solution is put 40 DEG C of people's Constant Temp. Oven constant temperature 5h.Get three small beakers, in bottom each 20 respectively by three kinds of effervescent tablets, after accurately weighing, be placed in and contain the NaCl exsiccator of supersaturated solution (the uncovered placement of weighing botle), preserve in 40 DEG C of constant temperature, after 4h, weigh once, and calculate moisture absorption percentage rate (%).
1.3.4.2 the mensuration of weight differential
Tablet, according to following method inspection, should conform with the regulations.
Inspection technique is got 20 of test samples, and accurately weighed gross weight is tried to achieve after average sheet weight, more accurate respectively
The weight of weighed every, every weight and the comparison of designation card heavy phase (without the heavy tablet of designation card, with average sheet anharmonic ratio), by the regulation in showing, what exceed limit test of weight variation must not be more than 2, and must not have 1 times of 1 overrun.
1.3.4.3 the mensuration of disintegration
Unless otherwise specified, check according to inspection technique disintegration (annex XII A), should conform with the regulations.The inspection method of disintegration is defined as: get 6 and split in 250mL beaker (inside filling 200mL water), water temperature is 15 DEG C～25 DEG C, there is numerous air-bubble to emit, in the time that the gas around tablet or fragment stops overflowing, tablet should dissolve or be dispersed in water, left without the granule of assembling.Unless otherwise specified, each all should disintegrate in 5min.If any 1 disintegrate completely, should get 6 retrials, all should conform with the regulations.
2 results and analysis
The extraction purification condition of 2.1 functional components is optimized
1647.167g Changshan grapefruit corium farinosum end, after 95% ethanol extraction three times, obtains oil-like extracts 500mL, and grease is used respectively after distilled water, 20%, 40%, 60%, 80% and 95% ethanol elution, after rotary evaporation, obtain solid, total amount is 73.3g, and crude product yield is 4.45%(table 4).Result can be found out simultaneously, and except distilled water, the solid of 40% ethanol elution is maximum, accounts for 21.3%.And the solid masses that 80% and 95% concentration ethanol eluant solution gets off is minimum, account for respectively 0.9% left and right.
The amount of the each concentration ethanol eluting of table 5 solid
*-alphabetical similarities and differences represent statistical discrepancy (small letter P<0.05, capitalization P<0.01)
80% ethanol elution is the highest containing flavonoid class material concentration as can be seen from Table 5, is secondly 40% and 60% ethanol elution, and 20% ethanol elution liquid hold-up is minimum.And for limonin, 40% and 80% ethanol elution liquid hold-up is the highest, be secondly 60% ethanol elution, 20% ethanol elution liquid hold-up is minimum.From total content, 40% ethanol elution liquid hold-up is the highest, and 80% ethanol elution takes second place, and minimum is 20% eluent.
The absorbance at wavelength place is being measured in the each concentration ethanol eluate of table 6
*-alphabetical similarities and differences represent statistical discrepancy (small letter P<0.05,, capitalization P<0.01)
Comprehensive the above results, can find out, the condition suggestion of extracting flavonoid and limonin material in Changshan grapefruit peel is: peel grinds after drying, and uses 95% ethanol extraction, and the rear macroporous resin chromatography of using, uses 40% ethanol elution, and crude product yield is 0.94%.
2.2 Changshan grapefruit flavonoid class and limonin content analysis
2.2.1 flavones ingredient
Table 7 Flavonoid substances assay result
As can be seen from Table 7, the Flavonoid substances total amount that Changshan grapefruit peel obtains by 40%, 60% and 80% ethanol elution reaches 742mg/kg.In the experiment of the people's such as Zhao Li Hu Benxiang Bullus Notholirionis Bulbuliferi Determination Method of Flavone Content research, from Bullus Notholirionis Bulbuliferi, extracting the total flavones amount obtaining is 14.045mg/kg.From Changshan grapefruit, extract the average general flavone content obtaining far above the content that extracts the total flavones obtaining from Bullus Notholirionis Bulbuliferi.From different ethanol concentration elute effect, 40% ethanol elution effect the best.
2.2.2 limonin constituents
Table 8 limonin substances assay result
As can be seen from Table 8, the limonin substances total amount that Changshan grapefruit peel obtains by 20%, 40%, 60% and 80% ethanol elution reaches 0.95%.And limonin extraction process and bacteriostatic activity research thereof in the people's such as Li Biao pomelo peel, the extraction ratio of result gained limonin is 6.08%, be significantly higher than the average extraction ratio of the limonin substances extracting in Changshan grapefruit, reflection Changshan grapefruit and the difference of conventional Fructus Citri grandis on limonin substances content.
From eluate, flavonoid and limonin substances be containing taking temperature by (table 7 and 8), the main eluting limonin substances of 40%, 60% and 80% ethanol.From both always taking temperature, effective ingredient purity 86%-99%.
2.3 Changshan grapefruit flavonoid class and the depression effect of limonin to pancreatic lipase activity
Table 9 is different ethanol elution things inhibitory action to pancreatic lipase activity.Result shows, it is active different that the pancreatic lipase of different ethanol concentration eluate suppresses, and the suppression ratio of 20% ethanol elution thing is the highest, reaches 146%, 60%, the suppression ratio of 80% and 90% ethanol elution thing is respectively 54.7%, 33.3% and 113.6%.This is because because flavonoid class material in different concentration ethanol eluate is different with citrin class material proportion and active there are differences of the pancreatic lipase of flavonoid class material and citrin class material inhibition caused.Must, result preliminary proof Changshan grapefruit there is stronger pancreatic lipase and suppress active, there is certain effect for reducing blood fat.
The maximum inhibition comparison of six kinds of eluate solution of table 9 to pancreatic lipase
2.4 effervescent tablet product forming techniques are optimized
2.4.1 the different proportion research of citric acid and natrium carbonicum calcinatum in effervescent tablet
The different proportioning test evaluation of result of table 10 adjuvant
In effervescent tablet, citric acid and sodium carbonate total amount account for 45% as can be seen from Table 10, and citric acid: when sodium carbonate is 1.6:1, tabletting effect is better.
2.4.2 the optimization of preparation condition
2.4.2.1 extract and various adjuvant were pulverized to 80 mesh sieves, soda acid mixes separately granulates, dry at different temperature, and after being dried, mix in soda acid source, pulverizes and under 6Mpa pressure, carry out tabletting.Obtain effervescent tablet.Effervescent tablet under different baking temperatures is carried out to the experiment of hydroscopicity.
The comparison of the different baking temperature hydroscopicity of table 11 medicament
As can be seen from Table 11,40 DEG C of dry rear gained effervescent tablet hydroscopicities are lower.
2.4.2.2 extract and various adjuvant were pulverized to 80 mesh sieves, soda acid mixes separately granulates, dry at 40 DEG C, and after being dried, mix in soda acid source, pulverizes, and carries out tabletting under different pressure.Obtain effervescent tablet.
Table 12 pressure different-effect is evaluated
Check according to inspection technique disintegration (annex XII A), each all should disintegrate in 5min, in conjunction with tabletting situation, as can be seen from Table 12: when tabletting pressure is 6Mpa, tabletting effect and disintegration time are better.
2.4.2.3 different pressures and the effervescent temperature evaluation of test result on end product quality impact
Extract and various adjuvant were pulverized to 80 mesh sieves, and soda acid mixes separately granulates, dry at 40 DEG C, and after being dried, mix in soda acid source, pulverizes, and carries out tabletting under different pressure.Obtain effervescent tablet.
Design water temperature is 15 DEG C, 20 DEG C, 35 DEG C water temperatures during for effervescent, carries out orthogonal experiment, and tabletting effect and effervescent effect to effervescent tablet are evaluated.
Table 13 different pressures and the effervescent temperature evaluation of test result on end product quality impact
Associative list 12,13 can obtain, and tabletting pressure adopts 6Mpa effect better, and meanwhile, when effervescent tablet water temperature should be greater than 15 DEG C, effervescent is effective.
Comprehensive three time preparation technologies probe into experiment, and we select citric acid and sodium carbonate total amount in effervescent tablet to account for 45%, and citric acid: sodium carbonate is 1.6:1,40 DEG C for baking temperature, 6Mpa be tabletting pressure.
2.4.3 quality testing evaluation
2.4.3.1 detect disintegration
Get 6 effervescent tablets and split in 250mL beaker (inside filling 200mL water), water temperature is 20 DEG C, records disintegration.Result is as table 14.
Table 14 effervescent tablet finished product detects disintegration
2.4.3.2 weight differential evaluation of result
Get 20 of effervescent tablet finished products, accurately weighed gross weight, tries to achieve after average sheet weight, more accurate respectively
The weight of weighed every, every weight and the comparison of designation card heavy phase (without the heavy tablet of designation card, with average sheet anharmonic ratio), result is as shown in Table 15.
Table 15 effervescent tablet finished weight difference results is evaluated
Can be obtained by table 15, end product quality meets the requirements
2.4.4 preliminary product development
While preparing effervescent tablet, take soda acid separately to granulate, it is that citric acid is made acid source that adjuvant is selected, and sodium carbonate is alkali source, and dextrin is diluent, and dehydrated alcohol is binding agent, and PEG-4000 is lubricant.Extract and relevant auxiliary materials are first crossed to 80 orders, wherein, 0.3g extract powder, 1.66g citric acid, 1.2g dextrin are mixed, with 0.135g dehydrated alcohol binding agent the most, 24 orders are granulated; In addition 0.3g extract powder, 1.04g citric acid, 1.2g dextrin are mixed, with 0.135g dehydrated alcohol binding agent the most, 24 orders are granulated.Respectively two kinds of granulations all being put into 40 DEG C of thermostatic drying chambers and be dried, after being dried, soda acid is mixed, add 0.03gPEG-4000, grind, after making fully to mix, is under 6Mpa, to carry out tabletting at pressure, obtains 15 of effervescent tablets.
3 discuss
3.1 the mensuration of flavonoid and limonin
3.1.1 the selection of solvent
Before the assay experiment of carrying out flavonoid and limonin substances, first to select suitable dissolution with solvents eluate.
In methanol, dehydrated alcohol, 95% ethanol, select eluate dissolubility higher as solvent, the relatively dissolubility of eluate in each solvent, selects dehydrated alcohol as solvent.Like this, both avoid the waste of solute, economized on resources, and also can improve the accuracy of experiment.
3.1.2 developer preparation
In assay experiment, need to use corresponding developer.
Adjust developer preparation program, and strictly follow now with the current principle and test.
3.2 determination of activity
3.2.1 mating of substrate and enzyme
In determination of activity experiment, first selected pancreatic lipase as determination of activity index enzyme, corresponding substrate is olive oil
3.2.2 the substrate solution of different schemes preparation affects enzyme activity
Substrate is olive oil, can not dissolve each other with pancreatic lipase solution.Probe into the compound method of different substrate solutions and pancreatic lipase solution, carry out the experiment of ultraviolet absorptivity mensuration, probe into the impact on lipase activity.Preparation program is a certain amount of n-hexane dissolution of substrate olive oil, in a certain amount of pancreatic lipase, adds normal hexane, then adds appropriate arabic gum, till presenting emulsion state to solution.
3.3 preparations shaping techniques
3.3.1 finished product hygroscopicity
The easy moisture absorption of medicine after molding, after effervescent tablet water suction itself, soda acid can react, and affects preparation end product quality.External environmental factor, in the time that external environment condition humidity is larger, also can have corresponding impact to medicine.Also have the upper not tight problem of sealing of some packagings, these all can make the medicine moisture absorption.
Analyze after reason, while considering preparation, adopt wet granulation, in adjuvant, the existence of moisture, on the hygroscopic impact of medicine, is taked different baking temperatures, relatively hydroscopicity after granulation.In conjunction with twice experimental result, determine that finished product prepares scheme.
3.4 process optimization
3.4.1 extract ungrease treatment
after application of sample, first wash with water.Macroporous resin the macromolecular substances such as water soluble polysaccharide, phlegmatic temperament is not adsorbed or absorption affinity a little less than, water can be by its eccysis, can make extract obtain certain purification.
Ethanol extraction contains a large amount of volatile oil compositions, if directly use D101 macroporous resin eluting, more serious to the damage ratio of macroporous resin, and loading just needs regeneration for 3 times afterwards.Therefore, ethanol extraction first need be carried out to defat, the petroleum ether of same volume extracts, and repeats after 5 times, lower floor's extract is left standstill in fume hood to 30min, and guarantee petroleum ether is removed completely.
Get the grease 5mL of pretreatment gained in separatory funnel, the petroleum ether that adds same volume extracts, and repeats after 5 times, lower floor's extract is left standstill in fume hood to 30min, and guarantee petroleum ether is removed completely, makes extract ungrease treatment.
Claims (6)
1. the preparation method of the effervescent tablet of Changshan grapefruit peel marc extract, is characterized in that comprising following processing step:
1) take each raw material according to following weight proportion
Changshan grapefruit peel marc extract powder 5～15%, citric acid and sodium carbonate 40～50%, dextrin 30～50%, dehydrated alcohol 2～8%, PEG-4000 0.2～1%, described citric acid: the weight ratio of sodium carbonate is 1.6:1;
2) get above-mentioned each raw material and cross 80 mesh sieves, Changshan grapefruit peel marc extract powder is evenly divided into two parts to be mixed with citric acid and sodium carbonate respectively, in Acid-Base System, add respectively dextrin to do filler, using dehydrated alcohol as binding agent, 24 orders are granulated and are carried out separately granulation of soda acid;
3) soda acid granulation being put into 40～70 DEG C of thermostatic drying chambers is dried; after being dried; soda acid is granulated and mixed; add the PEG-4000 of described weight proportion; grind; after it is fully mixed, under pressure 3～10Mpa, carry out tabletting, obtain the effervescent tablet of Changshan grapefruit peel marc extract.
2. the preparation method of the effervescent tablet of Changshan grapefruit peel marc extract as claimed in claim 1, is characterized in that described Changshan grapefruit peel marc extract powder makes by following steps:
A) get fresh Changshan grapefruit peel marc shred successively, 60 DEG C dry and pulverization process, obtain powder;
B) get the powder 95% alcoholic solution reflux that step 1) obtains and carry out three extractings, 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, obtain oil-like extracts;
C) get step 2) oil-like extracts that obtains adds petroleum ether to carry out ungrease treatment, and oil-like extracts and petroleum ether by volume 1:1 mix and extract, and take off a layer extract volatilization petroleum ether and obtain extract after defat after extraction;
D) after extracting degreasing, extract utilizes D101 type macroporous resin to carry out column chromatography, with the ethanol elution of concentration 20～80%, collects eluent, and eluent revolves steaming, pulverizes to obtain Changshan grapefruit peel marc extract powder.
3. the preparation method of the effervescent tablet of Changshan grapefruit peel marc extract as claimed in claim 1, is characterized in that taking each raw material by Changshan grapefruit peel marc extract powder 7～12%, citric acid and sodium carbonate 42～48%, dextrin 35～45%, dehydrated alcohol 3～6% and PEG-4000 0.4～0.8% in described step 1).
4. the preparation method of the effervescent tablet of Changshan grapefruit peel marc extract as claimed in claim 1, is characterized in that taking each raw material by Changshan grapefruit peel marc extract powder 10%, citric acid and sodium carbonate 45%, DEXTRIN %, dehydrated alcohol 4.5%, PEG-4000 0.5% in described step 1).
5. the preparation method of the effervescent tablet of Changshan grapefruit peel marc extract as claimed in claim 1, is characterized in that in described step 3), thermostatic drying chamber bake out temperature is 40 DEG C.
6. the preparation method of the effervescent tablet of Changshan grapefruit peel marc extract as claimed in claim 1, is characterized in that described step 3) tabletting pressure is 6Mpa.
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