CN103610010B - Fabrication method of pepper oleoresin microcapsule - Google Patents
Fabrication method of pepper oleoresin microcapsule Download PDFInfo
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- CN103610010B CN103610010B CN201310567607.3A CN201310567607A CN103610010B CN 103610010 B CN103610010 B CN 103610010B CN 201310567607 A CN201310567607 A CN 201310567607A CN 103610010 B CN103610010 B CN 103610010B
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- 235000008184 Piper nigrum Nutrition 0.000 title claims abstract description 157
- 235000002566 Capsicum Nutrition 0.000 title claims abstract description 155
- 239000006002 Pepper Substances 0.000 title claims abstract description 155
- 235000016761 Piper aduncum Nutrition 0.000 title claims abstract description 155
- 235000017804 Piper guineense Nutrition 0.000 title claims abstract description 155
- 239000008601 oleoresin Substances 0.000 title claims abstract description 138
- 239000003094 microcapsule Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 244000203593 Piper nigrum Species 0.000 title description 134
- 241000722363 Piper Species 0.000 claims abstract 23
- 239000007788 liquid Substances 0.000 claims description 69
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 31
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 28
- 239000000661 sodium alginate Substances 0.000 claims description 28
- 235000010413 sodium alginate Nutrition 0.000 claims description 28
- 229940005550 sodium alginate Drugs 0.000 claims description 28
- 239000003995 emulsifying agent Substances 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 20
- 239000000284 extract Substances 0.000 claims description 18
- 230000001112 coagulating effect Effects 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
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- 238000003756 stirring Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 80
- 239000000463 material Substances 0.000 abstract description 28
- 230000008569 process Effects 0.000 abstract description 21
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000002137 ultrasound extraction Methods 0.000 abstract description 6
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- 238000012545 processing Methods 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000005345 coagulation Methods 0.000 abstract 2
- 230000002542 deteriorative effect Effects 0.000 abstract 1
- 238000005453 pelletization Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 77
- 239000001894 piper nigrum l. oleoresin black Substances 0.000 description 48
- 238000012360 testing method Methods 0.000 description 39
- 239000001163 piper nigrum l. oleoresin white Substances 0.000 description 35
- 238000002474 experimental method Methods 0.000 description 29
- 230000000694 effects Effects 0.000 description 26
- 238000013461 design Methods 0.000 description 24
- 239000001110 calcium chloride Substances 0.000 description 22
- 229910001628 calcium chloride Inorganic materials 0.000 description 22
- 239000011162 core material Substances 0.000 description 21
- 238000010992 reflux Methods 0.000 description 14
- 230000004044 response Effects 0.000 description 14
- 239000002904 solvent Substances 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000013401 experimental design Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 206010011732 Cyst Diseases 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 238000009835 boiling Methods 0.000 description 6
- 208000031513 cyst Diseases 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 239000000341 volatile oil Substances 0.000 description 5
- 239000004480 active ingredient Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- MXXWOMGUGJBKIW-YPCIICBESA-N piperine Chemical compound C=1C=C2OCOC2=CC=1/C=C/C=C/C(=O)N1CCCCC1 MXXWOMGUGJBKIW-YPCIICBESA-N 0.000 description 4
- 229940075559 piperine Drugs 0.000 description 4
- WVWHRXVVAYXKDE-UHFFFAOYSA-N piperine Natural products O=C(C=CC=Cc1ccc2OCOc2c1)C3CCCCN3 WVWHRXVVAYXKDE-UHFFFAOYSA-N 0.000 description 4
- 235000019100 piperine Nutrition 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000002481 ethanol extraction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 235000013614 black pepper Nutrition 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 206010019133 Hangover Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 239000000783 alginic acid Substances 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 208000001130 gallstones Diseases 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000001931 piper nigrum l. white Substances 0.000 description 1
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- 230000008023 solidification Effects 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a fabrication method of a pepper oleoresin microcapsule. According to the method, the pepper oleoresin microcapsule is prepared by the following processes: firstly, extracting pepper oleoresin by adopting an ultrasonic wave in an assisting manner, and then pelletizing by an orifice-coagulation bath process. The extraction rate of the pepper oleoresin can be improved by ultrasonic-assisted extraction; the pepper oleoresin can be microencapsulated by the microcapsule fabricated by the orifice-coagulation bath process under a low-temperature condition; volatilization, decomposition and deterioration of the pepper oleoresin in the fabrication process are reduced; meanwhile, a good wall-forming material can form a film to embed the pepper oleoresin, so that the pepper oleoresin is isolated from an external environment, and damages of external factors such as light, oxygen and heat are reduced. By synthesis of the fabrication method, the extraction rate of the pepper oleoresin can be improved; a pepper oleoresin product can be effectively prevented from deteriorating in quality; the microencapsulation technology can be effectively applied to deep processing of pepper.
Description
Technical field
The invention belongs to technical field of agricultural product process, be specifically related to a kind of preparation method of pepper oleoresin microcapsules.
Background technology
Pepper is one of vegetable material of first dietotherapeutic announced of the Ministry of Public Health of China.Pepper can treat the various disease conditions such as poor appetite, diarrhoea, sore are swollen, gall stone, cancer.In pepper, chemical composition is numerous, and wherein main active ingredient is pipering and pepper essential oil.Pepper oleoresin is the leaching pasty masses by organic solvent, pepper powder being extracted to final gained, it comprises pungent excitor substance total in pepper and fragrance ingredient, and fragrance and taste compare balance, suitable directly adding in food directly eats as flavouring or after processing.Pepper oleoresin main component is pipering and pepper essential oil, and pipering is shown in that light easily decomposes, and pepper essential oil is heated volatile, and oxidizable, if lack good safeguard measure pepper oleoresin to be easy to deterioration, loses original quality.
Microcapsules technology, in solid, gas or the liquid utilizing macromolecular material that is natural or synthesis to be protected by needs is wrapped in, forms technology that is translucent or sealed Cellophane microcapsules.Microcapsule particle size controls at micrometer range, and its particle diameter is between 1-1000 μm, and microcapsule wall material dissolves, melts or break under given conditions, and core can discharge, by controlling the controlled Release of core material speed of the damaged speed of wall material.Therefore, extract pepper oleoresin in pepper by organic extraction process, and by microcapsules technology, pepper oleoresin is made microcapsules, the fine quality of maintenance pepper oleoresin that can be good.The preparation method of microcapsules is a lot, and wherein orifice-coagulating bath method is applicable to the preparation of oil substances microcapsules.Orifice-coagulating bath method utilizes the syringe of small-bore to instill in another kind of filmogen after being mixed with filmogen emulsification by core, and two kinds of filmogens react, and forms fine and close reticular membrane, in being wrapped in by core.
Summary of the invention
The object of this invention is to provide a kind of preparation method of pepper oleoresin microcapsules, the method is in conjunction with measures such as ultrasonic assistant optimization extraction, orifice-coagulating bath method microcapsules making, simple, less investment, be convenient to promote the use of, be suitable for use of large-scale production.。
The preparation method of a kind of pepper oleoresin microcapsules of the present invention first extracts pepper oleoresin with ultrasonic assistant, then obtain pepper oleoresin microcapsules with orifice-coagulating bath method granulation.
Specifically comprise the following steps:
(1) ultrasonic assistant extracts: by solid-liquid ratio 1:20(gmL
-1), in pepper powder, add absolute ethyl alcohol, lixiviate 55-60min at ultrasonic power is 230-240W, 65-70 DEG C, by extract by aperture 80-120 μm of filter paper vacuum filtration; After gained filtrate rotary evaporated to dryness, be placed in vacuum drying chamber, at 45-50 DEG C, dry under vacuum 130-133pa condition, obtain pepper oleoresin;
(2) pepper oleoresin emulsion is prepared: by pepper oleoresin and sodium alginate soln mass ratio 1:3, pepper oleoresin is joined 2.5% sodium alginate soln, add 0.2% emulsifier tween 80 simultaneously, stir at 50-55 DEG C, mix, mixing speed is 500r/min; Obtain pepper oleoresin emulsion;
(3) orifice-coagulating bath method granulation: coagulating bath (2-2.5% calcium chloride solution) is placed on magnetic stirring apparatus with 500r/min mixing speed and stirs, simultaneously by above-mentioned pepper oleoresin emulsion syringe instillation coagulating bath, drip speed 120/min, form microcapsules, these microcapsules solidify 30min in coagulating bath;
(4) pepper oleoresin microcapsules are obtained through separation, rinsing, vacuum drying again.
In the present invention, ultrasonic assistant extracts the recovery rate that can improve pepper oleoresin; Orifice-coagulating bath legal system makes microcapsules can under cryogenic by pepper oleoresin microencapsulation, reduce the volatilization of pepper oleoresin in manufacturing process, decomposition, go bad, simultaneously good wall-forming materials film forming can embed pepper oleoresin, itself and external environment are separated, decreases the destruction of the extraneous factors such as light, oxygen, heat.These inventions comprehensive, can improve the recovery rate of pepper oleoresin, effectively prevent pepper oleoresin quality deterioration, make microcapsules technology effectively can be applied to the deep processing of pepper.
Accompanying drawing explanation
Fig. 1 different solvents is on the impact of pepper oleoresin recovery rate.
Fig. 2 solid-liquid ratio is on the impact of pepper oleoresin recovery rate.
Fig. 3 reflux temperature is on the impact of pepper oleoresin recovery rate.
Fig. 4 extraction time is on the impact of pepper oleoresin recovery rate.
During Fig. 5, m-solid-liquid ratio reciprocation is on the impact of black pepper oleoresin extraction effect.
Fig. 6 temperature-solid-liquid ratio reciprocation is on the impact of black pepper oleoresin extraction effect.
Fig. 7 Time-temperature reciprocation is on the impact of black pepper oleoresin extraction effect.
The impact of Fig. 8 temperature-solid-liquid ratio reciprocation dialogue pepper oleoresin extraction effect.
The impact of m-solid-liquid ratio reciprocation dialogue pepper oleoresin extraction effect during Fig. 9.
The impact of Figure 10 Time-temperature reciprocation dialogue pepper oleoresin extraction effect.
Figure 11 solid-liquid ratio is on the impact of pepper oleoresin recovery rate.
Figure 12 extraction time is on the impact of pepper oleoresin recovery rate.
Figure 13 Extracting temperature is on the impact of pepper oleoresin recovery rate.
Figure 14 ultrasonic power is on the impact of pepper oleoresin recovery rate.
Figure 15 pipering calibration curve.
Figure 16 black pepper oleoresin microcapsules microphotograph (200 times).
Figure 17 is white pepper oleoresin microcapsule microphotograph (200 times).
Detailed description of the invention
Before further describing the specific embodiment of the invention, should be understood that protection scope of the present invention is not limited to following specific specific embodiments; It is also understood that the term used in the embodiment of the present invention is to describe specific specific embodiments, instead of in order to limit the scope of the invention; Embodiment one: the preparation of pepper oleoresin microcapsules
(1) dry: new fresh pepper is placed in air dry oven 48-52 DEG C and dries 48h;
(2) pulverize: the pepper after oven dry is pulverized with pulverizer, then cross 100 mesh sieves;
(3) ultrasonic assistant extracts: get appropriate pepper powder and be placed in tool plug conical flask, absolute ethyl alcohol is added by solid-liquid ratio 1:20, shake up, standing 1h is placed in ultrasonic unit, Modulating Power is 230-240W, lixiviate 55-60min at 65-70 DEG C, by extract by aperture 80-120 μm of filter paper vacuum filtration;
(4) vacuum drying: after gained filtrate rotary evaporated to dryness, be placed in vacuum drying chamber, at 45-50 DEG C, dry under vacuum 130-133pa condition, obtain pepper oleoresin;
(5) prepare pepper oleoresin emulsion: pepper oleoresin in mass ratio 1:3 joins 2.5% sodium alginate soln, add 0.2% emulsifier tween 80 simultaneously, stir at 50-55 DEG C, mix, mixing speed is 500r/min;
(6) orifice-coagulating bath method granulation: coagulating bath (2-2.5% calcium chloride solution) is placed on magnetic stirring apparatus with 500r/min mixing speed and stirs, simultaneously by above-mentioned pepper oleoresin emulsion syringe instillation coagulating bath, drip speed 120/min, form microcapsules, these microcapsules solidify 30min in coagulating bath;
(7) be separated: by the above-mentioned coagulating bath containing microcapsules by aperture 1-3 μm Filter paper filtering, collect wet microcapsules;
(8) rinsing: use clear water rinsing microcapsules 2-3 time, until show the calcium chloride solution of noresidue;
(9) vacuum drying: the wet microcapsules collected are placed in vacuum drying chamber, at 45-50 DEG C, is dried under vacuum 130-133pa condition and dryly obtains pepper oleoresin microcapsules.
Embodiment two: pepper oleoresin Study on extraction
1 condensing reflux extraction method
1.1 pepper oleoresin extraction process flow processs
Pepper → 50 DEG C baking 48h → pulverized 100 mesh sieves → refluxing extraction → suction filtration → filtrate concentrating → concentrate vacuum drying → pepper oleoresin
Pepper dries 48h under being placed in baking oven 50 DEG C of conditions, pulverizes and crosses 100 mesh sieves, obtaining pepper powder.Get appropriate pepper powder in 250mL flask, add a certain amount of organic reagent, connect condensation reflux unit, be placed in thermostat water bath, at a certain temperature lixiviate, extract suction filtration.Gained filtrate rotary evaporated to dryness final vacuum is dry, is pepper oleoresin.Pepper oleoresin is weighed, calculates recovery rate.
1.2 pepper oleoresin recovery rates calculate
1.3 single factor experiment designs
Carry out single factor experiment with solvent kind, extraction time, Extracting temperature, solid-liquid ratio 4 factors for influence factor, method is as follows:
Consider the impact of Extraction solvent: accurately took the pepper powder 5.000g of 100 mesh sieves in boiling flask, be that 1:16 adds absolute ethyl alcohol, methyl alcohol, ethyl acetate, acetone respectively by solid-liquid ratio, be placed in the thermostat water bath refluxing extraction 4.0h of 50 DEG C, then filter, and the water-bath being placed in 40 DEG C is concentrated into dry, weighs and calculate recovery rate after cooling.Often parallel three times of group test.
Consider the impact of solid-liquid ratio: accurately took the pepper powder 5.000g of 100 mesh sieves in boiling flask, be that 1:4,1:8,1:12,1:16,1:20 add absolute ethyl alcohol by solid-liquid ratio, be placed in the thermostat water bath refluxing extraction 4.0h of 50 DEG C, then filter, and the water-bath being placed in 40 DEG C is concentrated into dry, cooling calculates recovery rate after weighing.Often parallel three times of group test.
Consider the impact of Extracting temperature: accurately took the pepper powder 5.000g of 100 mesh sieves in boiling flask, be that 1:16 adds ethanol solution according to solid-liquid ratio, be placed in the water-bath refluxing extraction 4.0h of 40,50,60,70,80 DEG C respectively, then filter, and the thermostat water bath being placed in 40 DEG C is concentrated into dry, cooling calculates recovery rate after weighing.Often parallel three times of group test.
Consider the impact of extraction time: accurately took the pepper powder 5.000g of 100 mesh sieves in boiling flask, be that 1:16 adds ethanol solution by solid-liquid ratio, the thermostat water bath being placed in 50 DEG C respectively refluxing extraction 2.0,3.0,4.0,5.0,6.0h, then filter, and the water-bath being placed in 40 DEG C is concentrated into dry, cooling calculates recovery rate after weighing.Often parallel three times of group test.
1.4 response surface experiments designs
On single factor experiment basis, according to Box-Behnken center combination design principle, with pepper oleoresin recovery rate for response, design Extracting temperature, extraction time, the test of solid-liquid ratio 3 factor 3 horizontal respone surface analysis.Experimental design is in table 1.
Table 1 response surface experiments designs
| Level | Solid-liquid ratio/gmL -1 | Temperature/DEG C | Time/h |
| -1 | 1:12 | 60 | 4 |
| 0 | 1:16 | 70 | 5 |
| 1 | 1:20 | 80 | 6 |
2 ultrasonic assistant extract
2.1 pepper oleoresin extraction process flow processs
Pepper → 50 DEG C baking 48h → pulverized 100 mesh sieves → ultrasonic assistant extraction → suction filtration → filtrate concentrating → concentrate vacuum drying → pepper oleoresin
Pepper dries 48h under being placed in baking oven 50 DEG C of conditions, pulverizes and crosses 100 mesh sieves, obtaining pepper powder.Get appropriate pepper powder in 250mL tool plug conical flask, add a certain amount of absolute ethyl alcohol, shake up, leave standstill, treat that 1h is placed in ultrasonic cleaner, lixiviate at a certain temperature, extract suction filtration.Gained filtrate rotary evaporated to dryness final vacuum is dry, is pepper oleoresin.Weigh to pepper oleoresin, calculate recovery rate, computational methods are shown in 1.2.
2.2 single factor experiment designs
Carry out single factor experiment with extraction time, Extracting temperature, solid-liquid ratio, ultrasonic power 4 factors for influence factor, method is as follows:
Consider the impact of solid-liquid ratio: accurately took the pepper powder 5.000g of 100 mesh sieves in beaker, be that 1:10,1:15,1:20,1:25,1:30 add absolute ethyl alcohol by solid-liquid ratio, be placed in the supersonic wave cleaning machine that temperature is 50 DEG C, ultrasonic power is 160W, ultrasonic extraction 50min, then filter, and the water-bath being placed in 40 DEG C is concentrated into dry, weighs and calculate recovery rate after cooling.Often parallel three times of group test.
Consider the impact of extraction time: accurately took the pepper powder 5.000g of 100 mesh sieves in beaker, be that 1:20 adds absolute ethyl alcohol by solid-liquid ratio, be placed in the supersonic wave cleaning machine that temperature is 50 DEG C, ultrasonic power is 160W, respectively ultrasonic extraction 30,40,50,60,70min, then filter, and the water-bath being placed in 40 DEG C is concentrated into dry, weighs and calculate recovery rate after cooling.Often parallel three times of group test.
Consider the impact of Extracting temperature: accurately took the pepper powder 5.000g of 100 mesh sieves in beaker, be that 1:20 adds absolute ethyl alcohol by solid-liquid ratio, be placed in the supersonic wave cleaning machine that temperature is respectively 30,40,50,60,70 DEG C, ultrasonic power is 160W, ultrasonic extraction 50min, then filter, and the water-bath being placed in 40 DEG C is concentrated into dry, weighs and calculate recovery rate after cooling.Often parallel three times of group test.
Consider the impact of ultrasonic power: accurately took the pepper powder 5.000g of 100 mesh sieves in beaker, be that 1:20 adds absolute ethyl alcohol by solid-liquid ratio, be placed in the supersonic wave cleaning machine that temperature is respectively 50 DEG C, ultrasonic power is respectively 160,200,240,280,320W, ultrasonic extraction 50min, then filter, and the water-bath being placed in 40 DEG C is concentrated into dry, weighs and calculate recovery rate after cooling.Often parallel three times of group test.
2.3 Orthogonal Experiment and Design
On single factor experiment basis, adopt orthogonal experiment to be optimized pepper oleoresin ultrasound assisted extraction technique, carry out L with extraction time, Extracting temperature, solid-liquid ratio, ultrasonic power for factor
9orthogonal test.Experimental factor level is in table 2.
Table 2 Orthogonal Experiment and Design factor level and encoded radio
| Level | Solid-liquid ratio/gmL -1 | Temperature/DEG C | Time/min | Ultrasonic power/W |
| 1 | 1:15 | 50 | 40 | 200 |
| 2 | 1:20 | 60 | 50 | 240 |
| 3 | 1:25 | 70 | 60 | 280 |
Table 2 is the water-glass of black pepper oleoresin orthogonal test.
Table 3 Orthogonal Experiment and Design factor level and encoded radio
| Level | Solid-liquid ratio/gmL -1 | Temperature/DEG C | Time/min | Ultrasonic power/W |
| 1 | 1:20 | 30 | 50 | 160 |
| 2 | 1:25 | 40 | 60 | 200 |
| 3 | 1:30 | 50 | 70 | 240 |
Table 3 is the water-glass of white pepper oleoresin orthogonal test.
3 results and analysis
3.1 condensing reflux extraction methods
3.1.1 different solvents is on the impact of pepper oleoresin recovery rate
As seen from Figure 1, different solvents is different to the extraction effect of pepper oleoresin.For two kinds of pepper oleoresins, be all that methyl alcohol recovery rate is the highest, be secondly absolute ethyl alcohol, acetone, the recovery rate of ethyl acetate is minimum.For same solvent, the recovery rate of black pepper oleoresin is apparently higher than white pepper oleoresin.But consider that methyl alcohol has certain toxicity, and ethanol does not have toxicity, and the yield of ethanol is also higher, therefore, test all selects ethanol to be Extraction solvent.
3.1.2 solid-liquid ratio is on the impact of pepper oleoresin recovery rate
As seen from Figure 2, the recovery rate of black pepper oleoresin is apparently higher than white pepper oleoresin, and along with the increase of solid-liquid ratio, two kinds of pepper oleoresin yield raise all gradually, when solid-liquid ratio is lower than 1:16, black pepper oleoresin recovery rate increasing degree is greater than white pepper oleoresin, and substantially all reach maximum both when 1:16, after this solid-liquid ratio is increased, pepper oleoresin yield remains unchanged substantially, this may be due to when 1:16, two kinds of pepper oleoresin fully strippings in ethanol, reach dynamic equilibrium, continue to increase ethanol and can not improve yield, therefore test determines that solid-liquid ratio is 1:16.
3.1.3 Extracting temperature is on the impact of pepper oleoresin recovery rate
As seen from Figure 3, along with the rising of temperature, two kinds of pepper oleoresin yield also increase thereupon, and this may be because the diffusion coefficient of Extraction solvent increases along with temperature rising, thus extraction rate is accelerated, and extraction efficiency raises greatly.Reach 60 DEG C, black pepper oleoresin is along with the rising of temperature, recovery rate increase is comparatively obvious, and white pepper oleoresin increases slowly, close to recovery rate when 60 DEG C, these may be different due to the composition of two kinds of pepper oleoresins, in 60 DEG C of place black peppers, certain material distinctive is leached out, recovery rate is caused to increase obviously, and not containing this material in white pepper, so recovery rate keeps stable.Consider that temperature continues to raise the composition that may destroy in pepper oleoresin, increase production cost, the maximum temperature therefore tested all is chosen as 80 DEG C.
3.1.4 extraction time is on the impact of pepper oleoresin recovery rate
As seen from Figure 4, when the time is identical, the recovery rate of black pepper oleoresin is apparently higher than white pepper oleoresin, and extraction time is directly proportional to pepper oleoresin yield, reach 5h upon extracting, continue time expand, the yield of pepper oleoresin can not be significantly improved.This may due at the extraction initial stage, and two kinds of pepper oleoresins are along with the continuous stripping of prolongation of time, but after reaching certain hour, the stripping of pepper oleoresin is abundant, reaches balance, and continuing time expand does not affect substantially on extraction effect.Consider simultaneously and shorten the production cycle, therefore all select 6h to be the optimum extraction time.
3.1.5 black pepper oleoresin optimal extraction technology experimental design
According to single factor experiment result, adopt Box-Behnken center combination experimental design principle, with black pepper oleoresin recovery rate for response, choosing solid-liquid ratio (A), Extracting temperature (B) and extraction time (C) is experimental factor, carry out 3 factor 3 horizontal respone face Optimum Experiments, experimental design and the results are shown in Table 4.
Table 4 experimental design and result
| Tested number | A | B | C | Recovery rate/% |
| 1 | 0 | 0 | 0 | 10.908 |
| 2 | 1 | 0 | 1 | 10.805 |
| 3 | 1 | 0 | -1 | 10.565 |
| 4 | -1 | 0 | -1 | 10.252 |
| 5 | -1 | -1 | 0 | 10.434 |
| 6 | 0 | 0 | 0 | 10.828 |
| 7 | 0 | -1 | -1 | 10.012 |
| 8 | -1 | 0 | 1 | 10.788 |
| 9 | 0 | 0 | 0 | 10.902 |
| 10 | 1 | -1 | 0 | 10.588 |
| 11 | 0 | 1 | -1 | 10.765 |
| 12 | 0 | 0 | 0 | 10.879 |
| 13 | 0 | -1 | 1 | 10.748 |
| 14 | 0 | 1 | 1 | 10.976 |
| 15 | 1 | 1 | 0 | 10.902 |
| 16 | -1 | 1 | 0 | 10.742 |
| 17 | 0 | 0 | 0 | 10.839 |
Utilize Design Expert (version8.05) software his-and-hers watches 4 data to carry out multiple regression matching, obtain even experiment design:
Y=10.8712+0.0805A+0.20038B+0.21537C+1.5*10-3AB-0.07AC-0. 13125BC-0.11373A
2-0.090975B
2-0.15497C
2, in equation, Y represents black pepper oleoresin recovery rate, and A, B, C represent solid-liquid ratio, Extracting temperature, extraction time respectively.
The variance analysis of regression model is as table 5
Table 5 variance analysis
| Soruces of variation | Quadratic sum | The free degree | All square | F value | P value | Conspicuousness |
| Model | 1.05 | 9 | 0.12 | 32.47 | <0.0001 | ** |
| A | 0.052 | 1 | 0.052 | 14.48 | 0.0067 | ** |
| B | 0.32 | 1 | 0.32 | 89.71 | <0.0001 | ** |
| C | 0.37 | 1 | 0.37 | 103.64 | <0.0001 | ** |
| AB | 9.000E-006 | 1 | 9.000E-006 | 2.514E-003 | 0.9614 | Not remarkable |
| AC | 0.022 | 1 | 0.022 | 6.12 | 0.0426 | * |
| BC | 0.069 | 1 | 0.069 | 19.24 | 0.0032 | ** |
| A 2 | 0.054 | 1 | 0.054 | 15.21 | 0.0059 | ** |
| B 2 | 0.035 | 1 | 0.035 | 9.73 | 0.0169 | * |
| C 2 | 0.10 | 1 | 0.10 | 28.24 | 0.0011 | ** |
| Residual error | 0.025 | 7 | 3.581E-003 | |||
| Lose and intend error | 0.020 | 3 | 6.599E-003 | 5.01 | 0.0767 | Not remarkable |
| Pure error | 5.267E-003 | 4 | 1.317E-003 | |||
| Summation | 1.07 | 16 | ||||
| R 2=0.9766 | RAdj 2=0.9465 |
Note: " * * " P value is less than 0.01 for difference highly significant; " * " P value is less than 0.05 for significant difference.
As can be seen from Table 5, this model P value is less than 0.05, and significantly, losing and intending error is 0.0767, is greater than 0.05, not significantly, illustrates that this regression equation is better to test fitting degree.Once item A, B, C all reaches highly significant level; Mutual item BC highly significant, AC is remarkable; Quadratic term A
2, C
2highly significant, B
2significantly.Can be released by the F value size of 3 influence factors, 3 factors on the sequence that black pepper oleoresin yield affects size are: extraction time > Extracting temperature > solid-liquid ratio.Meanwhile, coefficient of determination R
2=0.9766, show that this equation can explain the change of the response of 97.66%, test error is less, therefore can extract test with this model to black pepper oleoresin and carry out analysis and prediction.The reciprocation of each factor is shown in Fig. 5-7.
In Fig. 5-7, shape analysis extraction time of each 3D surface chart and circle of equal altitudes, solid-liquid ratio and Extracting temperature are on the impact of pepper oleoresin recovery rate, and the steep of 3D curved surface can reflect that whether the reciprocation between Different factor is remarkable; Isocontour shape also can reflect that whether reciprocation between two factors is remarkable, and contour more levels off to ellipse, shows that two factor reciprocations are more remarkable, then not remarkable on the contrary.From Fig. 5-7, the reciprocation of extraction time and solid-liquid ratio is little on response impact, and whole curved surface is smoother, and contour levels off to circle, and pepper oleoresin yield is greater than solid-liquid ratio by the impact of extraction time; The change of reciprocation on response of Extracting temperature and solid-liquid ratio does not almost affect, and curved surface is level and smooth, and contour shape is close to circle, and pepper oleoresin yield is greater than solid-liquid ratio by the impact of Extracting temperature; The reciprocation of extraction time and Extracting temperature is to the obvious effect of response, and curved surface is very steep, and contour shape is close to ellipse, and pepper oleoresin yield is subject to the impact of time slightly larger than Extracting temperature.From response surface software analysis, at A=0.29, B=0.94, C=0.23, namely solid-liquid ratio is 1:17.2, and Extracting temperature is 79.4 DEG C, and when extraction time is 5.22h, pepper oleoresin can obtain maximum extracted rate, can reach 11.0% in theory.
3.1.6 white pepper oleoresin optimal extraction technology experimental design
According to single factor experiment result, adopt Box-Behnken center combination experimental design principle, with white pepper oleoresin recovery rate for response, choosing solid-liquid ratio (A), Extracting temperature (B) and extraction time (C) is experimental factor, carry out 3 factor 3 horizontal respone face Optimum Experiments, experimental design and the results are shown in Table-6.
Table 6 experimental design and result
| Tested number | A | B | C | Recovery rate/% |
| 1 | 0 | 0 | 0 | 10.201 |
| 2 | 0 | 0 | 0 | 10.14 |
| 3 | 1 | 0 | -1 | 9.954 |
| 4 | 1 | -1 | 0 | 9.951 |
| 5 | 0 | 0 | 0 | 10.206 |
| 6 | 0 | 0 | 0 | 10.168 |
| 7 | 0 | -1 | -1 | 10.012 |
| 8 | -1 | 0 | 1 | 10.108 |
| 9 | 1 | 0 | 1 | 10.111 |
| 10 | 0 | -1 | -1 | 9.436 |
| 11 | 0 | 0 | 0 | 10.414 |
| 12 | 1 | 1 | 0 | 10.255 |
| 13 | -1 | 0 | -1 | 9.679 |
| 14 | 0 | 1 | -1 | 10.058 |
| 15 | 0 | -1 | 1 | 10.061 |
| 16 | -1 | -1 | 0 | 9.83 |
| 17 | 0 | 1 | 0 | 10.261 |
Utilize Design Expert (version8.05) software his-and-hers watches 6 data to carry out multiple regression matching, obtain even experiment design:
Y=10.1658+0.080375A+0.16338B+0.080375C+0.03075AB-0.068AC-0.1055BC-0.072525A
2-0.081525B
2-0.13027C
2, in equation, Y represents black pepper oleoresin recovery rate, and A, B, C represent solid-liquid ratio, Extracting temperature, extraction time respectively.
3.1.7 the variance analysis of regression model
Table 7 variance analysis
| Soruces of variation | Quadratic sum | The free degree | All square | F value | P value | Conspicuousness |
| Model | 0.72 | 9 | 0.08 | 19.44 | 0.0004 | ** |
| A | 0.052 | 1 | 0.052 | 12.62 | 0.0093 | ** |
| B | 0.21 | 1 | 0.21 | 52.13 | 0.0002 | ** |
| C | 0.25 | 1 | 0.25 | 61.02 | 0.0001 | ** |
| AB | 3.782E-003 | 1 | 3.782E-003 | 0.92 | 0.3686 | Not remarkable |
| AC | 0.018 | 1 | 0.018 | 4.52 | 0.0712 | Not remarkable |
| BC | 0.045 | 1 | 0.045 | 10.87 | 0.0132 | * |
| A 2 | 0.022 | 1 | 0.022 | 5.41 | 0.053 | Not remarkable |
| B 2 | 0.028 | 1 | 0.028 | 6.83 | 0.0347 | * |
| C 2 | 0.071 | 1 | 0.71 | 17.45 | 0.0042 | ** |
| Residual error | 0.029 | 7 | 4.096E-003 | |||
| Lose and intend error | 0.022 | 3 | 7.488E-003 | 4.82 | 0.0813 | Not remarkable |
| Pure error | 6.209E-003 | 4 | 1.552E-003 | |||
| Summation | 0.75 | 16 | ||||
| R 2=0.9615 | RAdj 2=0.9121 |
Note: " * * " P value is less than 0.01 for difference highly significant; " * " P value is less than 0.05 for significant difference.
As can be seen from Table 7, this model P value is less than 0.05, and significantly, losing and intending error is 0.0813, is greater than 0.05, not significantly, illustrates that this regression equation is better to test fitting degree.Can be released by the F value size of 3 influence factors, the sequence that 3 factor dialogue pepper oleoresin yield affect size is: extraction time > Extracting temperature > solid-liquid ratio, the same with black pepper oleoresin, once item A, B, C also reaches highly significant level; Compared with black pepper oleoresin, mutual item BC becomes significantly from highly significant, and AB phase keeps not remarkable, and AC phase becomes significantly from highly significant; And quadratic term is except A
2become not remarkable from highly significant, other is all identical with black pepper oleoresin.Coefficient of determination R
2=0.9615, show that this equation can explain the change of the response of 96.15%, although a little less than 97.66%, test error is less, therefore can extract test with this model dialogue pepper oleoresin and carry out analysis and prediction.The reciprocation of each factor is shown in Fig. 8-10.
Fig. 8-10 shows the effect diagram of each factor reciprocation dialogue pepper oleoresin extraction effect, can find out, smoothly, contour is close to circle for Extracting temperature and extraction solid-liquid ratio interaction figure curved surface, visible reciprocation is very little, and white pepper oleoresin yield is greater than solid-liquid ratio by the impact of Extracting temperature; Solid-liquid ratio and time interaction figure curved surface are comparatively steep, and contour shape is ellipticity, show the obvious effect of their reciprocation dialogue pepper oleoresin recovery rate, and the influence degree of extraction time is greater than solid-liquid ratio; Extraction time and Extracting temperature interaction diagram curved surface steeper than the curved surface of other interaction diagrams, contour sub-elliptical shape, its reciprocation visible is stronger, and dialogue pepper oleoresin recovery rate influence degree is comparatively large, and white pepper oleoresin yield is subject to the impact of time slightly larger than Extracting temperature.From response surface software analysis, at A=0.73, B=1, C=0.08, namely solid-liquid ratio is 1:18.9, and Extracting temperature is 80 DEG C, and when extraction time is 5.08h, white pepper oleoresin can obtain maximum extracted rate, can reach 10.291% in theory.
3.1.8 optimum process condition checking
In order to the feasibility of auth response face method, at black pepper oleoresin optimum extraction condition, (solid-liquid ratio is 1:17.2, Extracting temperature is 79.4 DEG C, extraction time is 5.22h) under carry out 3 parallel tests, the mean value of the black pepper oleoresin recovery rate finally obtained is 10.982%, substantially meet with theoretical value, this model accurately and reliably as seen, utilizes this model to carry out in practice predicting it is feasible.
At white pepper oleoresin optimum extraction condition, (solid-liquid ratio is 1:18.9, Extracting temperature is 80 DEG C, extraction time is 5.08h) under carry out 3 parallel tests, the white pepper oleoresin recovery rate mean value finally obtained is 10.282%, substantially identical with theoretical value, this model visible accurately and reliably, utilizes this model to carry out in practice predicting it is feasible.
3.2 ultrasonic assistant extraction methods
3.2.1 solid-liquid ratio is on the impact of pepper oleoresin recovery rate
As seen from Figure 11, along with the increase of solid-liquid ratio, two kinds of oleoresin recovery rates all present first rise after downward trend, and during identical solid-liquid ratio black pepper oleoresin recovery rate apparently higher than white pepper oleoresin.When solid-liquid ratio reaches 1:20, two kinds of oleoresin recovery rates all reach the highest, and black pepper oleoresin recovery rate declines obviously afterwards, white pepper oleoresin kept stable.This may due to when solid-liquid ratio reaches 1:20, and oleoresin is fully stripping, reaches poised state, continue to increase solvent and can not dissolve more oleoresin, and too much solvent causes the prolongation of precipitation time, the volatilization of low boiling point component in oleoresin may be caused, reduce recovery rate.Consider, test determines that solid-liquid ratio is 1:20.
3.2.2 extraction time is on the impact of pepper oleoresin recovery rate
As seen from Figure 12, extraction time is more obvious on black pepper oleoresin impact.Along with the prolongation of extraction time, two kinds of oleoresin recovery rates all in first rising, rear downward trend.When ultrasonic time is 50min, both reach maximum, and the continuation increase time effectively can not increase recovery rate afterwards, and black pepper oleoresin decreases on the contrary.This may be because when 50min, the dissolving of oleoresin reaches poised state, and prolongation extraction time can make the material of some low boiling instability spill in air under hyperacoustic effect, thus causes the decline of recovery rate, and consider the production cycle, test determines that ultrasonic time is 50min.
3.2.3 Extracting temperature is on the impact of pepper oleoresin recovery rate
As seen from Figure 13, black pepper oleoresin recovery rate is greater than white pepper oleoresin, and the recovery rate of black pepper oleoresin is directly proportional to temperature simultaneously, and white pepper oleoresin recovery rate is in first increasing rear downward trend, and when temperature is 50 DEG C, extraction rate reached is to maximum.This is because along with the rising of temperature, the speed of solvent penetration and essential oil diffusion increases, and causes leaching rates to improve, and the high dissolving being of value to essential oil of temperature, so recovery rate finally raises.But for white pepper oleoresin, when temperature is higher than 50 DEG C, some volatile ingredient possible is unstable under the acting in conjunction of ultrasonic wave and temperature, easily overflows, thus reduces oleoresin recovery rate.
3.2.4 ultrasonic power is on the impact of pepper oleoresin recovery rate
As seen from Figure 14, ultrasonic power is similar to temperature to the impact that two kinds of oleoresins extract, black pepper oleoresin along with power increase recovery rate increase gradually, and white pepper oleoresin at ultrasonic power lower than in rising trend during 200W, decline gradually higher than after 200W.The shearing that the increase of ultrasonic power can make excusing from death produce and cavitation are strengthened, and are conducive to the destruction of cell membrane and the stripping of oleoresin, so black pepper oleoresin recovery rate is strengthened gradually; But after ultrasonic power reaches 200W, shear action and cavitation and temperature may produce certain comprehensive effect, destroy some composition in white pepper oleoresin or cause some composition in a solvent can not stabilizing dissolved, easy effusion, thus the recovery rate reducing white pepper oleoresin.
3.2.5 black pepper oleoresin Orthogonal Experiment and Design
Table 8 black pepper oleoresin process optimization orthogonal design and result
Black pepper oleoresin extracts orthogonal experiments in table 8, and the extreme difference size in table is C > D > A, B, and extreme difference is larger, when showing that this factor level changes, larger on result of the test impact.So four factors affects size order to oleoresin recovery rate: Extracting temperature > ultrasonic power > solid-liquid ratio, extraction time.Can be drawn by the size of average in table, optimum process condition is A
2b
3c
3d
2, be namely 1:20 at solid-liquid ratio, extraction time is 60min, and Extracting temperature is 70 DEG C, and when ultrasonic power is 240W, black pepper oleoresin exists maximum extracted rate in theory.Through parallel test checking, under optimum process condition, the actual black pepper oleoresin recovery rate that records is 11.08%, apparently higher than 9 tested numbers, proves that Optimum Experiment is reasonable.
3.2.6 white pepper oleoresin Orthogonal Experiment and Design
Table 9 white pepper oleoresin process optimization orthogonal design and result
Can be drawn by table 9, extreme difference size is C > D > B > A, so the impact of solid-liquid ratio dialogue pepper oleoresin recovery rate is minimum, Extracting temperature influence degree is maximum, identical with black pepper oleoresin.White pepper oleoresin optimal extract process is drawn: A by average size
3b
1c
3d
2, namely solid-liquid ratio is 1:30, and extraction time is 50min, and Extracting temperature is 50 DEG C, and when ultrasonic power is 200W, white pepper oleoresin exists maximum extracted rate in theory.Through parallel test checking, under optimum process condition, the actual white pepper oleoresin recovery rate that records is 10.35%, lower than black pepper oleoresin maximum extracted rate.This recovery rate, apparently higher than 9 tested numbers, proves that Optimum Experiment is reasonable.
4 brief summaries
The basis of screening organic reagent is optimized black pepper oleoresin ethanol extraction process, single factor experiment and the display of response surface optimization result, affecting size order to black pepper oleoresin yield is: extraction time > Extracting temperature > solid-liquid ratio.The black pepper oleoresin ethanol extraction process parameter optimized: solid-liquid ratio 1:17.2, Extracting temperature 79.4 DEG C, extraction time 5.22h, under this condition, the recovery rate of black pepper oleoresin is 10.982%.
Ultrasonic assistant method is adopted to extract pepper oleoresin, and adopt orthogonal test to be optimized, result of the test shows, and several factor is to the influence degree size order of black pepper oleoresin recovery rate: Extracting temperature > ultrasonic power > solid-liquid ratio, extraction time.Be 1:20 at solid-liquid ratio, extraction time is 60min, and Extracting temperature is 70 DEG C, and when ultrasonic power is 240W, black pepper oleoresin recovery rate is 11.08%, higher than condensing reflux extracts 10.982%.
Several factor dialogue pepper oleoresin yield affects size order: extraction time > Extracting temperature > solid-liquid ratio, the white pepper oleoresin ethanol extraction process parameter optimized: solid-liquid ratio is 1:18.9, Extracting temperature is 80 DEG C, extraction time is 5.08h, and under this condition, white pepper oleoresin can obtain maximum extracted rate 10.282%.
The influence degree size order of several factor dialogue pepper oleoresin recovery rate: Extracting temperature > ultrasonic power > extraction time > solid-liquid ratio.Be 1:30 at solid-liquid ratio, extraction time is 50min, and Extracting temperature is 50 DEG C, and when ultrasonic power is 200W, white pepper oleoresin exists maximum extracted rate: 10.35%, higher than condensing reflux method: 10.282%.
Contrast condensing reflux method and ultrasonic assistant method, two kinds of pepper oleoresins use recovery rate during ultrasonic assistant method optimum process condition all a little more than condensing reflux method, and the time is obviously less than condensing reflux method, production cycle can be greatly reduced, reduce cost, be thus more suitable for the extraction of pepper oleoresin.
Embodiment three: pepper oleoresin microcapsules preparation research
1 technological process
After the mixing of sodium alginate soln, calcium chloride solution and Tween 80, through orifice granulation, separation, rinsing, dry finished product.
2 key points for operation
The preparation of sodium alginate soln: take appropriate sodium alginate powder in 200mL beaker, adds a small amount of distilled water and stirs, continue to add distilled water and be stirred to dissolution homogeneity without bulky grain powder in 50 DEG C of water-baths, places 50min and solution is fully mixed.
Coagulating bath configures: the calcium chloride powder taking different amount, in 200mL beaker, adds appropriate distilled water, glass bar stirring and dissolving, is made into the calcium chloride solution of variable concentrations.
Pepper oleoresin emulsion configures: add sodium alginate soln by a certain percentage, calcium chloride solution and emulsifier tween 80, stirs at 50 DEG C to 60 DEG C, and mixing mixing, mixing speed is 500r/min.
Granulation: coagulating bath be placed on magnetic stirring apparatus with 500r/min mixing speed and stir, instills in coagulating bath by pepper oleoresin emulsion syringe simultaneously, drips speed control built in 120/min, form microcapsules.
Solidification is dry: microcapsules solidify 30min in coagulating bath, filters, and collects wet microcapsules, with clear water rinsing repeatedly, until the calcium chloride solution of surperficial noresidue, be placed in vacuum drying chamber dry.
3 embedding rates measure
In formula: A
1for the content of pipering in microcapsules; A
2for the content of pipering in pepper oleoresin before non-emulsification.
The mensuration of 4 content of piperine
Ultraviolet method is adopted to measure content of piperine.
The mensuration of content of piperine in 5 microcapsules
The microcapsules of drying are placed in mortar grind, cyst wall is destroyed, be transferred to beaker, add soaked in absolute ethyl alcohol, constantly stir with glass bar, filter, filter residue alcohol immersion, repeat above operation, until final filtrate is not containing pipering, merging filtrate, constant volume, with ultraviolet specrophotometer mensuration content of piperine wherein, calculate embedding rate.
6 Orthogonal Experiment and Design
According to trial test result, with sodium alginate content, core wall material proportioning, calcium chloride content and emulsifier content for influence factor, design L
9(3
4) orthogonal test.
6.1 sodium alginate content are on the impact of microcapsules
Fixing calcium chloride content 2%, core wall material proportioning is 1:3, emulsifier content 0.2%, and controlling sodium alginate content is 1%, 1.5%, 2%, 2.5%, 3% 5 gradient, and making microcapsules, take embedding rate as index, evaluates sodium alginate content to the impact of microcapsules.
6.2 core wall material proportionings are on the impact of microcapsules
Fixing sodium alginate content is 2%, and calcium chloride content is 2%, emulsifier content 0.2%, and controlling core wall material proportioning is 1:1,1:2,1:3,1:4,1:5 five gradients, and making microcapsules, take embedding rate as index, evaluates core wall material proportioning to the impact of microcapsules.
6.3 calcium chloride content are on the impact of microcapsules
Fixing sodium alginate content is 2%, and core wall material proportioning is 1:3, emulsifier content 0.2%, and controlling calcium chloride content is 1%, 1.5%, 2%, 2.5%, 3% 5 gradient, and making microcapsules, take embedding rate as index, evaluates calcium chloride content to the impact of microcapsules.
6.4 emulsifier contents are on the impact of microcapsules
Fixing control sodium alginate content is 2%, and calcium chloride content is 2%, core wall material proportioning is 1:3, and controlling emulsifier content is 0.1%, 0.15%, 0.2%, 0.25%, 0.3% 5 gradient, makes microcapsules, take embedding rate as index, evaluate emulsifier content to the impact of microcapsules.
6.5 orthogonal experiment factor level tables
Table 10 orthogonal test gauge outfit
7 results and analysis
7.1 pipering calibration curves
As shown in figure 15, in the scope of 0 to 16 μ g/mL, absorbance and pipering concentration linear, this equation y=0.1495x+0.0154, R
2=0.9994, correlation is good.
7.2 sodium alginate content are on the impact of microcapsules
Table 11 sodium alginate content is on the impact of pepper oleoresin microencapsulation
As shown in Table 11, black pepper oleoresin is similar with white pepper oleoresin, and along with the increase of sodium alginate content, microcapsules molding effect is become better and better, embedding rate first increases and then decreases.This is because when sodium alginate concentration is lower, the cyst wall of the microcapsules of formation is thinner, and mechanicalness is poor, and drying process easily makes cyst wall be destroyed, and reduces embedding rate; When concentration is higher, sodium alginate soln is thickness comparatively, not easily extrudes with detachable needle syringe, and easily causes hangover, forms irregular microcapsules, is unfavorable for the embedding of oleoresin.Consider, it is 2% comparatively suitable that sodium alginate content is chosen as.
7.3 core wall material proportionings are on the impact of microcapsules
Table 12 core wall material proportioning is on the impact of pepper oleoresin microencapsulation
Table 12 indicates different core wall material proportioning to the impact of microcapsules effect, as apparent from the table, the embedding effect of two kinds of oleoresins is substantially identical, along with the increase of wall material, the embedding of oleoresin takes the lead in increasing rear reduction, and when core wall ratio reaches 1:3, embedding rate reaches maximum.Cause the reason of this phenomenon may be wall material more time, cyst wall is thicker, and the active ingredient can wrapped up in capsule is less, adds cost; When wall material is less, the cyst wall of the microcapsules of formation is thinner, and in wall, active ingredient is easily separated out, and reduces embedding rate.Consider, it is comparatively suitable that core wall material proportioning is chosen as 1:3.
7.4 calcium chloride content are on the impact of microcapsules
Table 13 calcium chloride content is on the impact of pepper oleoresin microencapsulation
As can be seen from Table 13, the embedding rate impact of calcium chloride content on two kinds of oleoresin microcapsules is larger.Along with the increase of calcium chloride content, the molding effect of microcapsules is become better and better, but embedding rate is in the rear downward trend that first rises.This is because when calcium chloride content is less than 2%, the cyst wall that sodium alginate and calcium chloride are formed is thinner, easily impaired, is not easy to the parcel of active ingredient; When calcium chloride content is greater than 2%, embedding rate declines to some extent, but is totally more or less the same, and remains on more than 60%.But consider Cost Problems, simultaneously the excessive concentration of calcium chloride solution, obtained oleoresin microcapsule surface defines fine and close alginic acid calcium layer, be unfavorable for the drying of microcapsules, and mouthfeel is not good yet, thus calcium chloride content be chosen as 2% comparatively suitable.
7.5 emulsifier contents are on the impact of microcapsules
Table 14 emulsifier content is on the impact of pepper oleoresin microencapsulation
As can be seen from Table 14, the content of emulsifying agent does not have other factors obvious on microcapsules molding effect and embedding rate impact, along with the increase of emulsifier content, embedding rate presents ascendant trend by a small margin, substantially reach stable when content is 0.2%, this be due to emulsifier content lower time, pepper oleoresin and sodium alginate mixing and emulsifying are abundant not, are unfavorable for embedding; When emulsifier content reaches a certain amount of, core and wall material fully mix, and continue to increase emulsifier content and can not improve the degree of mixing of core wall material, and more than comprehensive, it is 0.2% comparatively suitable that emulsifier content is chosen as.
7.6 quadrature analysis
7.6.1 black pepper oleoresin microencapsulation Orthogonal Experiment and Design
Table 15 black pepper oleoresin micro-encapsulation technology optimizes orthogonal design and result
As shown in Table 15, with microcapsule embedded rate for index, overall merit extreme difference size, it is calcium chloride content > sodium alginate content > core wall material proportioning > emulsifier content that result shows each factor to microencapsulation influential effect degree size order, namely calcium chloride content has the greatest impact to microcapsule embedded rate, and emulsifier content is minimum on microcapsule embedded rate impact.Contrast average size can show that the optimised process of microcapsules is A
3b
3c
2d
2, namely calcium chloride content is 2.5%, and sodium alginate content is 2.5%, and emulsion content is 0.2%, and when core wall material proportioning is 1:3, the embedding rate of microcapsules exists theoretical maximum.With this understanding, through three parallel verified tests, final obtained microcapsules molding effect is better, and embedding rate reaches 73.32%, higher than 9 test group of orthogonal test.
7.6.2 white pepper oleoresin microcapsule Orthogonal Experiment and Design
Table 16 white pepper oleoresin microcapsule metallization processes optimizes orthogonal design and result
As shown in Table 16, white pepper oleoresin and black pepper oleoresin are extremely similar, and with microcapsule embedded rate for index, it is also having the greatest impact of calcium chloride content that overall merit extreme difference size result shows each factor effect size order, and the impact of emulsifier content is minimum.Contrast average size can show that the optimised process of microcapsules is A
3b
3c
2d
2, the same with black pepper oleoresin, there is theoretical maximum in the embedding rate of microcapsules under this technique.With this understanding, through three parallel verified tests, final obtained microcapsules molding effect is better, and embedding rate reaches 75.15%, and higher than 9 test group of Orthogonal Experiment and Design, and black pepper oleoresin closely.
7.6.3 the enlarged drawing of microcapsules under optimised process
As can be seen from Figure 16 and Figure 17, obtained microcapsules regular shape, molding effect is better.
8 brief summaries
(1) analyzed the Different factor affecting pepper oleoresin microencapsulation effect by single factor test and orthogonal optimization test, draw calcium chloride content and sodium alginate content to microencapsulation influential effect comparatively greatly, emulsifier content impact is less.
(2) find best micro capsule technology that is black, white pepper oleoresin by orthogonal optimization, be: calcium chloride content is 2.5%, sodium alginate content is 2.5%, and emulsion content is 0.2%, and core wall material proportioning is 1:3.
(3) orifice-coagulating bath method is a kind of low temperature Microencapsulation Method, for easily volatilizing under the high temperature conditions, decompose, the material of sex change, as pepper oleoresin, is a desirable Microencapsulation Method.
Claims (1)
1. a preparation method for pepper oleoresin microcapsules, is characterized in that, is first to extract pepper oleoresin with ultrasonic assistant, then obtains pepper oleoresin microcapsules with orifice-coagulating bath method granulation; Concrete steps are:
(1) ultrasonic assistant extracts
By 1g pepper powder: the solid-liquid ratio of 20mL ethanol, adds absolute ethyl alcohol in pepper powder, lixiviate 55-60min at ultrasonic power is 230-240W, 65-70 DEG C, by extract by aperture 80-120 μm of filter paper vacuum filtration; After gained filtrate rotary evaporated to dryness, be placed in vacuum drying chamber, at 45-50 DEG C, dry under vacuum 130-133pa condition, obtain pepper oleoresin;
(2) pepper oleoresin emulsion is prepared: by pepper oleoresin and sodium alginate soln mass ratio 1:3, pepper oleoresin is joined 2.5% sodium alginate soln, add 0.2% emulsifier tween 80 simultaneously, stir at 50-55 DEG C, mix, mixing speed is 500r/min; Obtain pepper oleoresin emulsion;
(3) orifice-coagulating bath method granulation: be that coagulating bath is placed on magnetic stirring apparatus with 500r/min mixing speed and stirs by 2-2.5% calcium chloride solution, simultaneously by above-mentioned pepper oleoresin emulsion syringe instillation coagulating bath, drip speed 120/min, form microcapsules, these microcapsules solidify 30min in coagulating bath;
(4) pepper oleoresin microcapsules are obtained through separation, rinsing, vacuum drying again.
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