CN102450648B - Extraction method for dietary fiber from citrus peel residues - Google Patents
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Abstract
The invention belongs to the technical fields of fruit and vegetable processing and comprehensive utilization of citrus, and specifically relates to a preparation method for extracting edible dietary fiber with high added value from citrus peel residues. According to the present invention, the following key technologies are optimized and screened to determine the extraction method for the dietaryfiber from the citrus peel residues, wherein the key technologies comprise: a pretreatment, fermentation conditions of the soluble dietary fiber, alkali extraction of the insoluble dietary fiber, andother related conditions. The extracted dietary fiber of the present invention maintains the physiological activity to the maximal degree. The extraction rate of the total dietary fiber from the citrus peel residues is 56.23-68.18%, and the purity of the extracted dietary fiber is high, and is 87.59-96.42%.
Description
Technical field
The invention belongs to garden stuff processing and oranges and tangerines comprehensive utilization technique field, be specifically related to a kind of edible dietary fiber that utilizes oranges and tangerines processing byproduct (citrus peel residue) to extract high added value, the present invention is optimized the alkaline process extraction conditions of the fermentation extraction conditions of wherein key technology such as preliminary treatment, soluble dietary fiber and insoluble diedairy fiber, has determined a kind of extracting method of dietary fiber from citrus peel residues.
Background technology
Oranges and tangerines are the maximum fruit of output in the world, and about 40% of world's orange yield is used to processing.The mandarine annual production is only second to Brazil, the U.S., occupies the 3rd in the world.At present, the major product of mandarine processing has orange blossom, syrup tangerine lobe can, oranges and tangerines jelly and jam, orange wine, oranges and tangerines preserved fruit, orange fruit vinegar etc.According to estimates, from the squeezing of juice class is produced, can obtain the citrus pulp about 50%, can obtain 25% orange peel in the can processing.In the world the application of oranges and tangerines pomace is mainly reflected in the following aspects now: the extraction of the compositions such as essential oil, pigment, pectin, dietary fiber, flavonoids, limonoid, the production of ethanol, fruit vinegar, orange peel beverage, natural clouding agent and feed, fertilizer etc.Domestic report was crossed from orange peel and is extracted mandarin oil, pectin, orange peel former times, food coloring and produce orange peel beverage etc. and utilize approach in recent years, but these utilize approach many because of product single, industrialization level is low, shortcoming (the Qiao Haiou etc. such as raw material availability is not high, secondary pollution is serious, the comprehensive utilization of orange peel. the Zhejiang Agriculture science, 2003,3:147-149).Therefore, the oranges and tangerines processing byproduct should be avoided environmental pollution to greatest extent as the with different levels reasonable comprehensive utilization of raw material, is the needs that meet the human resource sustainable development.The skin slag of accessory substance is as raw material in the oranges and tangerines processing, adopt advanced practical science and technology, take full advantage of and preserve the functional health ingredient of citrus peel residue, prepare high-quality dietary fiber from citrus peel residues, not only realized zero the discarding in the oranges and tangerines processing, resource has obtained adequately and reasonably utilizing, and has protected ecological environment, to optimizing the Citrus Industry structure, the added value tool that increases the oranges and tangerines processing industry is of great significance; And be that the resource optimization of other garden stuff processing accessory substances, rationally comprehensive utilization provide referential method.
The oranges and tangerines processing waste material accounts for 50% of fruit take pericarp, pomace and seed as main, contains many utilities, such as sugar, hemicellulose, cellulose, pectin, glycocide, essential oil and pigment.One of main path of citrus peel residue utilization centers on the extraction of its ingredient and launches, some emerging approach that utilize have also appearred in recent years, as the orange peel drying is made organic fertilizer, citrus peel meal can be used as the feed anticorrosion agent, alcohol extract after the orange peel baking can be used for excited beverage or as the substitute of coffee ﹠ tea, the white cortex of oranges and tangerines food fibre powder and lemon is used for boiling or drying sausage improves the sausage quality as a kind of functional additive.Skin slag utilization after the countries such as Brazil and the U.S. process oranges and tangerines mainly is the skin slag directly to be dried make animal feed and do not stay any discarded object, has realized the discarded object recycling.The experience of external oranges and tangerines processing industry developed country shows, citrus by-product is carried out rational exploitation and utilization, not only can improve the raw material comprehensive utilization ratio, reduce production costs, improve added value and economic benefit, and can environmental contamination reduction, this has become very important important step (Fernando Figuerola etal.Fiber concentrates from apple pomace and citrus peel as potential fiber source for good enrichment.FoodChemistry, 2005 (91): 395-401) in the modernized oranges and tangerines processing.
The preparation of dietary fiber from citrus peel residues and the search time of application are not long, nineteen eighty-three Braddock etc. are used for processing fiber to the white cortex of oranges and tangerines, and the extraction of cellulose, hemicellulose, pectin and lignin in orange exocarp, mesocarp, fruit juice cyst, chip and the seed is studied.Altomare in 1985 etc. have studied and have utilized the Citrus White cortex to make a kind of empty calory raising agent partly to substitute flour in the cake, fat and the component (Li Zhaohui such as sugared, Li Jian etc., the experimental study of Preparation of Water-soluble Food Cellulose With Enzyme. Beijing University of Technology's journal, 2004,30 (1): 45-48).The people's such as Porzio in 1992 result of study shows that capsule clothing chip and the broken juice born of the same parents of containing the thick pulp of part are a kind of good dietary sources.Y.Lario E. etc. then adopt simple physical method to make lemon diet fibers from the lemon juice processing byproduct, cleaning and dry technology have been estimated emphatically to the impact (Y.Lario of dietary fiber physico-chemical property, E et al.Preparation of high dietary fiber powder from lemon juice by-products.Innovative Food Science and Emerging Technologies, 2004 (5): 113-117).The bright and beautiful orange peel slag after to squeeze the juice such as Pan Ming, Wang Shikuan is as raw material, take physical method as the main dietary fiber that extracts, improved the ratio (Pan Ming of soluble dietary fiber and insoluble diedairy fiber, Wang Shikuan, brocade orange peel dregs diet fibre extracts research. Sichuan Light Chemical Engineering College's journal, 1999,12 (4): 54-58).2003, Liang Min etc. are take the swab skin as raw material, inquired into and adopted chemical method to extract and adopt respectively chemical method, enzyme process, chemical method and enzyme process combined techniques to extract the technique (Liang Min of insoluble diedairy fiber, Pan Yingming, from pomelo peel, extract the research of dietary fiber. Chemical Engineering Technology and exploitation, 2003,32 (6): 20-22).
The research of dietary fiber from citrus peel residues also is in the starting stage, does not have at present the example of practical application.Because its low pol, low fat, solubility and insoluble dietary fiber ratio are suitable, it is the desirable material of exploitation healthy food, can be widely used in various food, health products and the pharmaceutical products, main purpose is the dietary fiber amount of replenishing needed by human body, increases health care, improvement product special flavour, raising product quality and the added value etc. of product.Along with the raising of people's living standard and the fast development of food industry; fully utilize being rich in the functional components citrus peel residue; be not only the Important Action of preserving the ecological environment, improve especially the Citrus Industry chain, drive the new wind vane of the sound development of whole Citrus Industry.
Summary of the invention
The object of the invention is to break through the Pinch technology link of prior art, a kind of extracting method of dietary fiber from citrus peel residues is provided.The method comprises the extraction process of dietary fiber, inquires into different pretreatments baking temperature and grinding particle size to the impact of citrus peel residue water-soluble dietary fiber recovery rate, selects best pretreatment condition; Adopt chemistry-fermentation method to extract dietary fiber from citrus peel residues, Optimized Extraction Process is supported for the high-quality dietary fiber from citrus peel residues of a large amount of extractions provides theoretical.The present invention selects the citrus peel residue of different cultivars to ferment with different Trichoderma kinds, studies show that and select general cellulase-producing Trichoderma kind that the different cultivars citrus peel residue is fermented, all can reach better effects, expand some thinkings for screening from now on high yield dietary fiber citrus peel residue kind and efficient fermented bacterium.
The present invention realizes by following technical proposal:
A kind of extracting method of dietary fiber from citrus peel residues, its step is as follows:
1) select suitable citrusfruit for processing raw material;
2) mode of washing cleans fruit to adopt that clear water soaks, washes away etc.;
3) with centrifugal type juicing machine with step 2) the cleaning fruit squeeze the juice, collect fruit juice and skin slag;
4) with step 3) the skin slag manually go chopping behind the seed, its width is 3mm;
5) with step 4) the skin slag put into 40 ℃～60 ℃ dry 48h of electric heating constant-temperature blowing drying box, make the skin pulp water divide content to keep 5%～10%;
6) with step 5) broken mistake 40 orders of dry skin ground-slag～80 mesh sieves, obtain the citrus peel residue powder and pack in the freshness protection package, at room temperature be stored in the drier for subsequent use;
7) to step 6) skin ground-slag end 1: 5～1: the 25 adding distilled water of press solid-liquid ratio, be the 20min that sterilizes under the 103kPa at 121 ℃, pressure;
8) until step 7) skin slag cooling after, regulate original ph 6.0～10.0 with 0.1mol/LNaOH solution, access by volume 1%～5% wooden mould pityrosporion ovale (for example Trichoderma viride 13030 or healthy and free from worry wood mould 40505) suspension, at 24 ℃～36 ℃ lower shaken cultivation 24h～48h of temperature, keep rotating speed 160rpm;
9) with step 8) in after the skin slag sterilization, cooling after the fermentation, centrifugal 20min under rotating speed 4200rpm;
10) with step 9) supernatant liquor adding in 1: 4 by volume ethanol solution, centrifugal after the standing over night, abandoning supernatant, precipitation places vacuum drying chamber vacuum drying (40 ℃ of temperature, vacuum 80kPa), namely obtain the citrus peel residue soluble dietary fiber;
11) with step 9) middle centrifugation gained lower sediment, press solid-liquid ratio and added distilled water in 1: 5～1: 25, and regulate pH value to 7.0～11.0 with 0.1mol/LNaOH solution, suction filtration behind 50 ℃～90 ℃ lower stirring in water bath 60min～180min, filter residue carries out vacuum drying, namely obtains the citrus peel residue insoluble diedairy fiber;
12) with step 10), 11) in the dietary fiber that obtains collect, mix, pulverize, namely obtain dietary fiber from citrus peel residues.
The different condition of skin slag and granule size is dried in the present invention under lower temperature range by comparing citrus peel residue, on the impact of dietary fiber from citrus peel residues recovery rate, determined best pretreated temperature and grinding particle size.
The present invention has studied the impact of different fermentations condition on citrus peel residue soluble dietary fiber recovery rate, by L9 (3
4) orthogonal test determines optimum extraction process and condition.
The present invention has also studied the impact of different chemical condition on citrus peel residue insoluble diedairy fiber recovery rate, determines optimum extraction process and condition by variance analysis.
Good effect of the present invention is:
1) compared with prior art, the whole leaching process of the present invention all adopts relatively mild experimental condition, and do not have involving in of murder by poisoning or corrosive substance, this not only can make the dietary fiber that extracts farthest keep its physiologically active, also so that the dietary fiber of carrying has higher security.
2) dietary fiber recovery rate of the present invention is higher: according to surveying and determination, the recovery rate that extracts total dietary fiber from the limepeel slag can reach 56.23～68.18%.
3) the dietary fiber purity of the present invention's extraction is high, impurity is few, its purity 87.59%～96.42%.
4) method of extracting dietary fiber among the present invention is extracted soluble dietary fiber and insoluble diedairy fiber respectively with diverse ways, not only significantly improved extraction efficiency, and provides some thinkings for sophisticated category from now on prepares dietary fiber.
More detailed technical scheme sees that " specific embodiment " is described.
Description of drawings
Fig. 1: be the technological process that dietary fiber from citrus peel residues of the present invention extracts.
Fig. 2: different baking temperatures are on the impact of citrus peel residue soluble dietary fiber recovery rate.
Fig. 3: the different grain size size is on the impact of citrus peel residue soluble dietary fiber recovery rate.
Fig. 4: solid-liquid ratio is on the impact of limepeel slag soluble dietary fiber recovery rate.
Fig. 5: fermentation time is on the impact of limepeel slag soluble dietary fiber recovery rate.
Fig. 6: fermentation temperature is on the impact of limepeel slag soluble dietary fiber recovery rate.
Fig. 7: original ph is on the impact of limepeel slag soluble dietary fiber recovery rate.
Fig. 8: the different vaccination amount is on the impact of limepeel slag soluble dietary fiber recovery rate.
Fig. 9: extraction time is on the impact of bright and beautiful orange peel slag insoluble diedairy fiber recovery rate.
Figure 10: extract temperature to the impact of bright and beautiful orange peel slag soluble dietary fiber recovery rate.
Figure 11: solid-liquid ratio is on the impact of bright and beautiful orange peel slag insoluble diedairy fiber recovery rate.
Figure 12: original ph is on the impact of bright and beautiful orange peel slag insoluble diedairy fiber recovery rate.
The specific embodiment
Embodiment 1:
A kind of extracting method of bitter orange dietary fiber from citrus peel residues, its step is as follows:
1) selecting maturity is 90% and ripe consistent, and fruit appearance is disease-free, and the bitter orange of machinery-free damage (Songzi, Hubei Province is hoped spring flower fruit juice Co., Ltd oranges and tangerines base) fruit is for processing raw material;
2) the mode of washing cleaning fruit that adopts that clear water soaks, washes away etc., after squeezing the juice, collection fruit juice and skin slag;
3) with step 2) the skin slag manually go chopping behind the seed, its width is 3mm, put into 50 ℃ of dry 48h of electric heating constant-temperature blowing drying box after, pulverized 60 mesh sieves, in the freshness protection package of packing into, at room temperature be stored in the drier for subsequent use;
4) get step 3) skin ground-slag end 20g, be to add distilled water 100mL at 1: 5 by the ratio of feed liquid, be the 20min that sterilizes under the 103kPa at 121 ℃, pressure; After the sterilization cooling, regulate original ph 9.0 with 0.1mol/LNaOH solution, pityrosporion ovale suspension (Trichoderma viride 13030 bacterial strains of Trichoderma viride 13030 bacterial strains of ratio access 2% by volume, be purchased from Chinese industrial microorganism fungus kind preservation center, specifying information is seen the 1st part of data of other testimonial material sectional drawings), at 30 ℃ of lower shaken cultivation 48h, the maintenance rotating speed is 160rpm;
5) with step 4) in skin slag sterilization after the fermentation, be centrifugal 15min under the 4200rpm at rotating speed after cooling;
6) with step 5) supernatant liquor adding in 1: 4 by volume ethanol solution, centrifugal after the standing over night, abandoning supernatant, will be deposited in temperature is 40 ℃, vacuum is to carry out vacuum drying under the 80kPa, namely obtains the citrus peel residue water-soluble dietary fiber;
7) with step 6) in centrifugal gained lower sediment, ratio by feed liquid is 1: 15 adding distilled water, and regulate pH value to 10.0 with 0.1mol/LNaOH solution, suction filtration behind 80 ℃ of lower stirring in water bath 2h, filter residue places the vacuum drying chamber vacuum drying, and (temperature is 40 ℃, vacuum is 80kPa), namely obtain the citrus peel residue insoluble diedairy fiber;
8) with step 6), 7) in the dietary fiber that obtains collect, mix, pulverize, namely obtain dietary fiber from citrus peel residues.
Obtain 13.28g bitter orange dietary fiber from citrus peel residues after this technique, recovery rate is 66.39%, and its purity is 92.61%.
Embodiment 2:
A kind of extracting method of bitter orange dietary fiber from citrus peel residues, its step is as follows:
1) selecting maturity is 90% and ripe consistent, and fruit appearance is disease-free, and the bitter orange of machinery-free damage (Songzi, Hubei Province is hoped spring flower fruit juice Co., Ltd oranges and tangerines base) fruit is for processing raw material;
2) the mode of washing cleaning fruit that adopts that clear water soaks, washes away etc., after squeezing the juice, collection fruit juice and skin slag;
3) with step 2) the skin slag manually go chopping behind the seed, its width is 3mm, put into 50 ℃ of dry 48h of electric heating constant-temperature blowing drying box after, pulverized 60 mesh sieves, in the freshness protection package of packing into, at room temperature be stored in the drier for subsequent use;
4) get step 3) skin ground-slag end 20g, ratio by feed liquid adds distilled water 100mL at 1: 5, be the 20min that sterilizes under the 103kPa at 121 ℃, pressure, after the sterilization, regulate original ph 6.0 with 0.1mol/LNaOH solution, press the pityrosporion ovale suspension (Trichoderma viride 13030 bacterial strains are purchased from Chinese industrial microorganism fungus kind preservation center) of Trichoderma viride 13030 bacterial strains of (fermentation tank feed liquid and Trichoderma viride) volume ratio access 1%, at 27 ℃ of lower shaken cultivation 48h, the maintenance rotating speed is 160rpm;
5) with step 4) in skin slag sterilization after the fermentation, be centrifugal 20min under the 4200rpm at rotating speed after cooling;
6) with step 5) supernatant liquor adding in 1: 4 by volume ethanol solution, centrifugal after the standing over night, abandoning supernatant, being deposited in temperature down is 40 ℃, vacuum is to carry out vacuum drying under the 80kPa, namely obtains the citrus peel residue water-soluble dietary fiber;
7) with step 6) in centrifugal gained lower sediment, ratio by feed liquid adds distilled water at 1: 15, and regulate pH value to 7.0 with 0.1mol/LNaOH solution, suction filtration behind 50 ℃ of lower stirring in water bath 60min, filter residue places the vacuum drying chamber vacuum drying, and (temperature is 40 ℃, vacuum is 80kPa),, namely obtain the citrus peel residue insoluble diedairy fiber;
8) with step 6), 7) in the dietary fiber that obtains collect, mix, pulverize, namely obtain dietary fiber from citrus peel residues.
Obtain 11.25g bitter orange dietary fiber from citrus peel residues after this technique, recovery rate is 56.23%, and its purity is 87.59%.
Embodiment 3:
A kind of extracting method of bitter orange dietary fiber from citrus peel residues, its step is as follows:
1) selecting maturity is 90% and ripe consistent, and fruit appearance is disease-free, and the bitter orange of machinery-free damage (Songzi, Hubei Province is hoped spring flower fruit juice Co., Ltd oranges and tangerines base) fruit is for processing raw material;
2) the mode of washing cleaning fruit that adopts that clear water soaks, washes away etc., after squeezing the juice, collection fruit juice and skin slag;
3) with step 2) the skin slag manually go chopping behind the seed, its width is 3mm, put into 50 ℃ of dry 48h of electric heating constant-temperature blowing drying box after, pulverized 60 mesh sieves, in the freshness protection package of packing into, at room temperature be stored in the drier for subsequent use;
4) get step 3) skin ground-slag end 20g, ratio by feed liquid adds distilled water 500mL at 1: 25, be the 20min that sterilizes under the 103kPa at 121 ℃, pressure, after the sterilization, regulate original ph 10.0 with 0.1mol/LNaOH solution, press pityrosporion ovale suspension (Trichoderma viride 13030 bacterial strains of Trichoderma viride 13030 bacterial strains of (fermentation tank feed liquid and Trichoderma viride) volume ratio access 1%, be purchased from Chinese industrial microorganism fungus kind preservation center), at 33 ℃ of lower shaken cultivation 48h, the maintenance rotating speed is 160rpm;
5) with step 4) in skin slag sterilization after the fermentation, be centrifugal 20min under the 4200rpm at rotating speed after cooling;
6) with step 5) supernatant liquor adding in 1: 4 by volume ethanol solution, centrifugal after the standing over night, abandoning supernatant, being deposited in temperature down is 40 ℃, vacuum is to carry out vacuum drying under the 80kPa, namely obtains the citrus peel residue water-soluble dietary fiber;
7) with step 6) in centrifugal gained lower sediment, press solid-liquid ratio and add distilled water at 1: 25, and regulate pH value to 11.0 with 0.1mol/LNaOH solution, suction filtration behind 90 ℃ of lower stirring in water bath 180min, filter residue places the vacuum drying chamber vacuum drying, and (temperature is 40 ℃, vacuum is 80kPa), namely obtain the citrus peel residue insoluble diedairy fiber;
8) with step 6), 7) in the dietary fiber that obtains collect, mix, pulverize, namely obtain dietary fiber from citrus peel residues.
Obtain 13.64g bitter orange dietary fiber from citrus peel residues after this technique, recovery rate is 68.18%, and its purity is 96.42%.
Embodiment 4:
The extracting method of the orange dietary fiber from citrus peel residues of a kind of brocade, its step is as follows:
1) selecting maturity is 90% and ripe consistent, and fruit appearance is disease-free, and the brocade orange of machinery-free damage (Songzi, Hubei Province is hoped spring flower fruit juice Co., Ltd oranges and tangerines base) fruit is for processing raw material;
2) the mode of washing cleaning fruit that adopts that clear water soaks, washes away etc., after squeezing the juice, collection fruit juice and skin slag;
3) with step 2) the skin slag manually go chopping behind the seed, its width is 3mm, put into 50 ℃ of dry 48h of electric heating constant-temperature blowing drying box after, pulverized 60 mesh sieves, in the freshness protection package of packing into, at room temperature be stored in the drier for subsequent use;
4) get step 3) skin ground-slag end 20g press solid-liquid ratio adding in 1: 15 distilled water 300mL, be the 20min that sterilizes under the 103kPa at 121 ℃, pressure; After the sterilization cooling, regulate original ph 9.0 with 0.1mol/LNaOH solution, (healthy and free from worry wood is mould to access by volume 2% the mould pityrosporion ovale suspension of healthy and free from worry wood, bacterium numbering 40505, be purchased from Chinese industrial microorganism fungus kind preservation center, specifying information is seen the 2nd part of data of other testimonial material sectional drawings), at 30 ℃ of lower shaken cultivation 48h, the maintenance rotating speed is 160rpm;
5) with step 4) in skin slag sterilization after the fermentation, be centrifugal 15min under the 4200rpm at rotating speed after cooling;
6) with step 5) supernatant liquor adding in 1: 4 by volume ethanol solution, centrifugal after the standing over night, abandoning supernatant, being deposited in temperature down is 40 ℃, vacuum is to carry out vacuum drying under the 80kPa, namely obtains the citrus peel residue water-soluble dietary fiber;
7) with step 6) in centrifugal gained lower sediment, press solid-liquid ratio and add distilled water at 1: 15, and regulate pH value to 10.0 with 0.1mol/LNaOH solution, suction filtration behind 80 ℃ of lower stirring in water bath 2h, filter residue places the vacuum drying chamber vacuum drying, and (temperature is 40 ℃, vacuum is 80kPa), namely obtain the citrus peel residue insoluble diedairy fiber;
8) with step 6), 7) in the dietary fiber that obtains collect, mix, pulverize, namely obtain bright and beautiful orange dietary fiber from citrus peel residues.
Obtain 12.75g bitter orange dietary fiber from citrus peel residues after this technique, recovery rate is 63.77%, and its purity is 90.13%.General product cellulose bacterial classification is used in evidence such as healthy and free from worry wood is mould and Trichoderma viride, to dietary fiber from citrus peel residues enough preferably extraction effects can be arranged all, and Citrus Cultivars difference is not obvious.
Embodiment 5 (test example 1: different pretreatments is on the impact of citrus peel residue water-soluble dietary fiber recovery rate)
1 different baking temperature experimental pretreatment materials:
Brocade orange peel slag (brocade orange: fruit shape goose egg shape, its sisters' strain is " pioneer's orange ", fruit shape spheroidal, originate in Sichuan Province China Jiangjin City sweet orange class improved seeds (bud mutation kind), the '30s is selected, 60 to the seventies at Sichuan and Hubei spread, fresh fruit sugar peracid is high, be fit to eat raw after the storage or to be fit to processing juice processed) be the leftover bits and pieces that fresh fruit machinery deoils and squeezes the juice behind the capsule, hope spring flower fruit juice Co., Ltd available from Songzi City, Hubei Province, be cut into the filament that width is 3mm, be placed on respectively 40 ℃, 50 ℃, 60 ℃, pulverize behind the dry 48h under 70 ℃ and 80 ℃, cross 60 mesh sieves, at room temperature be stored in the drier for subsequent use.
2 different grain sizes size experimental pretreatment material:
Bright and beautiful orange peel slag is cut into the filament that width is 3mm, behind 50 ℃ of lower dry 48h, pulverizes, cross respectively 20 orders, 40 orders, 60 orders, 80 orders, 100 mesh sieves, at room temperature be stored in the drier for subsequent use.
The preparation of 3 bright and beautiful orange soluble dietary fibers:
Take by weighing the pretreated bright and beautiful orange peel ground-slag of 10g different condition end, add 150mL distilled water (solid-liquid ratio is 1: 15), after the cooling of sterilization skin slag, regulate pH value to 9.0, access by volume 2% Trichoderma viride pityrosporion ovale suspension (Trichoderma viride 13030 bacterial strains that reached stationary phase, be purchased from Chinese industrial microorganism fungus kind preservation center), be that 30 ℃, rotating speed are shaken cultivation 48h under the 160rpm in temperature; Sterilization, centrifugal (rotating speed is 4200rpm, and the time is 15min); Supernatant liquor ratio by volume adds ethanol solution at 1: 4, and is centrifugal after the standing over night, abandoning supernatant, and precipitation is carried out vacuum drying (temperature is 40 ℃, and vacuum is 80kPa), namely obtains bright and beautiful orange peel dregs water-soluble dietary fiber.
The mensuration of 4 bright and beautiful orange peel slag soluble dietary fibers:
Content with reference to the enzyme among the AOAC 991.43-gravimetric detemination soluble dietary fiber (SDF).
Accompanying drawing 2 is that different baking temperatures are on the impact of citrus peel residue water-soluble dietary fiber recovery rate.
Accompanying drawing 3 is that the different grain size size is on the impact of citrus peel residue soluble dietary fiber recovery rate.
As can be seen from Figure 2, preliminary treatment when bake out temperature is 50 ℃, impact on citrus peel residue water-soluble dietary fiber recovery rate is better than other bake out temperatures, and lower bake out temperature also can keep the activity of soluble dietary fiber preferably, so select 50 ℃ to be the preliminary treatment bake out temperature.
As can be seen from Figure 3, granularity also increases along with granularity increases the soluble dietary fiber recovery rate during less than 60 order, and after granularity surpassed 60 orders, the variation of soluble dietary fiber recovery rate was not obvious, is the preliminary treatment grinding particle size therefore select 60 orders.
Embodiment 6:(test example 2: the different fermentations condition is on the impact of citrus peel residue soluble dietary fiber recovery rate)
1 test material
Being test material at the limepeel slag of pulverizing 60 mesh sieves after 50 ℃ of lower oven dry (fresh fruit machinery deoil the leftover bits and pieces of squeezing the juice behind the capsule, hope spring flower fruit juice Co., Ltd available from Songzi City, Hubei Province).
2 test methods:
2.1 single factor experiment
After 50 ℃ of lower oven dry, to pulverize the limepeel slag of 60 mesh sieves as raw material, choose cultivation temperature, incubation time, solid-liquid ratio, original ph etc. the influential factor of citrus peel residue soluble dietary fiber recovery rate is carried out single factor experiment, determine its optimum range.
2.1.1 solid-liquid ratio is on the impact of limepeel slag soluble dietary fiber recovery rate
Limepeel ground-slag end is 1: 5,1: 10,1: 15,1: 20,1: 25 adding distilled water by the ratio of feed liquid respectively, be under the 103kPa behind the sterilization 20min at 121 ℃, pressure, regulate original ph 8.0 with 0.1mol/LNaOH solution, access by volume 2% Trichoderma viride pityrosporion ovale 13030 suspensions, (Trichoderma viride 13030 bacterial strains, be purchased from Chinese industrial microorganism fungus kind preservation center), at 30 ℃ of lower shaken cultivation 48h, the maintenance rotating speed is 160rpm; Centrifugal after skin slag sterilization after the fermentation, the cooling; Supernatant liquor added ethanol solution in 1: 4 by volume, after the standing over night, and centrifugal, abandoning supernatant, precipitation is carried out vacuum drying (temperature is 40 ℃, and vacuum is 80kPa), namely obtains limepeel slag soluble dietary fiber; The result as shown in Figure 4, the increase that the recovery rate of soluble dietary fiber changes with solid-liquid ratio increases gradually, recovery rate is the highest when the solid-liquid ratio degree is 1: 15, selected suitable solid-liquid ratio is 1: 15 (W/V).
2.1.2 fermentation time is on the impact of limepeel slag soluble dietary fiber recovery rate
Limepeel ground-slag end is pressed solid-liquid ratio and is added distilled water at 1: 15, ferments by different fermentations times such as 12h, 24h, 36h, 48h, 60h respectively, and the same 2.1.1 of other steps namely obtains limepeel slag soluble dietary fiber; The result as shown in Figure 5, the increase that the recovery rate of soluble dietary fiber changes with fermentation time increases gradually, recovery rate is the highest when fermentation 36h, continues subsequently fermentation, recovery rate descends to some extent, therefore selected suitable fermentation time is 36h.
2.1.3 fermentation temperature is on the impact of limepeel slag soluble dietary fiber recovery rate
Limepeel ground-slag end press solid-liquid ratio and is added distilled water at 1: 15, and by the different fermentations temperature cultivation 48h such as 24 ℃, 27 ℃, 30 ℃, 33 ℃, 36 ℃, the same 2.1.1 of other steps namely obtains limepeel slag soluble dietary fiber respectively; The result as shown in Figure 6, the increase that the recovery rate of soluble dietary fiber changes with fermentation temperature increases gradually, and recovery rate is the highest when fermentation temperature is 30 ℃, subsequently the continuation of fermentation temperature rise, recovery rate descends to some extent, therefore selected suitable fermentation temperature is 30 ℃.
2.1.4 original ph is on the impact of limepeel slag soluble dietary fiber recovery rate
Limepeel ground-slag end is pressed solid-liquid ratio and is added distilled water at 1: 15, and regulating respectively original ph is 6.0,7.0,8.0,9.0,10.0, and the same 2.1.1 of other steps namely obtains limepeel slag soluble dietary fiber; The result as shown in Figure 7, the increase that the recovery rate of soluble dietary fiber changes with original ph increases, when original ph recovery rate 9.0～10.0 time the highest, along with the continuation increase of pH value, recovery rate descends to some extent, therefore selected suitable original ph is 9.0.
2.1.5 the different vaccination amount is on the impact of limepeel slag soluble dietary fiber recovery rate
Limepeel ground-slag end is pressed solid-liquid ratio and is added distilled water at 1: 15, and by the Trichoderma viride pityrosporion ovale suspension of different amount volume ratios 1%, 2%, 3%, 4%, 5% access, the same 2.1.1 of other steps namely obtains limepeel slag soluble dietary fiber; The result as shown in Figure 8, the recovery rate of soluble dietary fiber changes increase with inoculum concentration and changes not obviously, and recovery rate is the highest when inoculum concentration is 2%, therefore selected suitable inoculum concentration is 2%.
2.2 orthogonal test
According to the single factor experiment result, on the factor (fermentation temperature, fermentation time, solid-liquid ratio, original ph etc.) that affects bitter orange soluble dietary fiber recovery rate, adopt L9 (34) orthogonal test to determine to extract optimum condition, Orthogonal Experiment and Design sees Table 1.The orthogonal experiments of extraction conditions and variance analysis see Table respectively 2, shown in the table 3.
Table 1 extraction conditions orthogonal test factor and level
Table 2 extracting condition orthogonal experiments
Table 3 analysis of variance table
Analyze by result's (table 2) and the results of analysis of variance (table 3) to orthogonal test, the extreme difference R that shows the B factor is maximum, therefore the impact of fermentation method extraction limepeel slag soluble dietary fiber is fermentation temperature the most significantly, next is solid-liquid ratio, fermentation time, initial pH is minimum on the impact of extraction effect, and four factors all reach the utmost point level of signifiance.According to the size of K value as can be known, the order of four factor pair recovery rate impacts is: fermentation temperature (B)＞fermentation time (A)＞original ph (D)＞solid-liquid ratio (C), the optimal conditions that fermentation method extracts limepeel slag soluble dietary fiber is A3B3C2D1, be that temperature is that 32 ℃, solid-liquid ratio are 1: 10, fermentation time is that 42h and initial pH are 9.0.Variance analysis shows: all conditions impact all reaches the utmost point level of signifiance, and wherein fermentation temperature and fermentation time have the greatest impact to recovery rate.
Embodiment 7:(test example 3: the different chemical condition is on the impact of citrus peel residue insoluble diedairy fiber recovery rate)
1 test material
By the optimum condition of implementing screening in 6, the bright and beautiful orange peel slag of namely pulverizing 60 mesh sieves after 50 ℃ of lower oven dry adds distilled water by solid-liquid ratio at 1: 10, regulate original ph 9.0 with 0.1mol/LNaOH solution after the sterilization, access by volume 2% Trichoderma viride 13030 bacterial strain pityrosporion ovale suspensions, at 32 ℃ of lower shaken cultivation 42h, the maintenance rotating speed is 160rpm; Centrifugal after skin slag sterilization after the fermentation, the cooling, supernatant liquor is used for extracting bright and beautiful orange peel dregs water-soluble dietary fiber, collects lower sediment as this test material.
The mensuration of 2 bright and beautiful orange peel slag insoluble diedairy fibers:
Test material is added distilled water by certain solid-liquid ratio, and regulate the pH value with 0.1mol/LNaOH solution, suction filtration behind the stirring in water bath certain hour at a certain temperature, filter residue places the vacuum drying chamber vacuum drying, and (temperature is 40 ℃, vacuum is 80kPa), namely obtain bright and beautiful orange peel slag insoluble diedairy fiber.
Content with reference to the enzyme among the AOAC991.43-gravimetric detemination insoluble diedairy fiber (IDF).
3 single factor experiments
Choose extraction time, extraction temperature, solid-liquid ratio, original ph etc. the influential factor of bright and beautiful orange peel slag insoluble diedairy fiber recovery rate is carried out single factor experiment, determine its optimum range.
3.1.1 extraction time is on the impact of bright and beautiful orange peel slag insoluble diedairy fiber recovery rate
Test material is pressed solid-liquid ratio add distilled water at 1: 15, and regulate pH value to 10.0 with 0.1mol/LNaOH solution, stir respectively 60min 50 ℃ of lower water-baths, 90min, 120min, 150min, suction filtration behind the 180min, filter residue places the vacuum drying chamber vacuum drying, and (temperature is 40 ℃, vacuum is 80kPa), namely obtain bright and beautiful orange peel slag insoluble diedairy fiber, the result as shown in Figure 9, the increase that the recovery rate of insoluble diedairy fiber changed with extraction time increases, after extraction time surpasses 120min, recovery rate changes not obvious, therefore selected suitable extraction time is 120min.
3.1.2 extract temperature to the impact of bright and beautiful orange peel slag soluble dietary fiber recovery rate
Test material is pressed solid-liquid ratio add distilled water at 1: 15,50 ℃ of different bath temperatures, 60 ℃, 70 ℃, 80 ℃, 90 ℃ are lower stir 120min after suction filtration, filter residue carries out vacuum drying, namely obtain bright and beautiful orange peel slag insoluble diedairy fiber, the result as shown in Figure 10, the recovery rate of insoluble diedairy fiber changes with the increase of extracting temperature and increases, therefore selected suitable extraction temperature is 80 ℃.
3.1.3 solid-liquid ratio is on the impact of bright and beautiful orange peel slag insoluble diedairy fiber recovery rate
Test material was added distilled water by different feed liquid than 1: 5,1: 10,1: 15,1: 20,1: 25, at 50 ℃ of lower water-bath 120min, the same 2.1.1 of other steps, namely obtain bright and beautiful orange peel slag insoluble diedairy fiber, the result as shown in Figure 11, the recovery rate of insoluble diedairy fiber changes with the increase variation of solid-liquid ratio not obvious, therefore selected suitable solid-liquid ratio is 1: 15.
3.1.4pH value is on the impact of bright and beautiful orange peel slag insoluble diedairy fiber recovery rate
Test material is regulated different pH values 7.0,8.0,9.0,10.0,11.0 with 0.1mol/LNaOH solution, at 50 ℃ of lower water-bath 120min, the same 2.1.1 of other steps, namely obtain bright and beautiful orange peel slag insoluble diedairy fiber, the result as shown in Figure 12, the increase that the recovery rate of insoluble diedairy fiber changes with the pH value increases, when the pH value is higher than 10.0, recovery rate descends on the contrary to some extent, therefore selected suitable pH value is 10.0.
3.2 variance analysis test
According to the single factor experiment result, the factor (extracting temperature, extraction time, solid-liquid ratio, pH value etc.) on affecting bright and beautiful orange insoluble diedairy fiber recovery rate adopts the variance analysis test to determine to extract optimum condition, and experimental factor and level design see Table 4.The results of analysis of variance of extraction conditions is shown in Table 5.
Table 4 extraction conditions experimental factor and level
Table 5 extraction conditions test variance analysis
By the results of analysis of variance (table 5) is analyzed, the extreme difference R that shows the B factor is maximum, therefore being to extract temperature the most significantly on the extraction effect impact of bright and beautiful orange peel slag insoluble diedairy fiber, secondly is pH value, solid-liquid ratio, and extraction time is minimum on the impact of extraction effect.According to the size of K value as can be known, the optimal conditions of the extraction of bright and beautiful orange peel slag insoluble diedairy fiber is A3B1C2D1, namely extraction time be 150min, extract temperature be 70 ℃, pH value be 10.0 and solid-liquid ratio be 1: 15.
Claims (1)
1. a citrus peel residue that derives from bitter orange or brocade orange prepares the method for dietary fiber, it is characterized in that following steps:
(1) obtains the skin slag after the bitter orange after will cleaning or bright and beautiful orange fresh fruit are squeezed the juice, manually go to put into the dry 48～72h of 50 ℃ of electric heating constant-temperature blowing drying boxes after seed, the chopping, make the skin pulp water divide content to 5～10%; With broken mistake 60 mesh sieves of the skin ground-slag of drying, obtain pretreated bitter orange or bright and beautiful orange peel ground-slag end;
(2) pretreated bitter orange or the bright and beautiful orange peel ground-slag end with step (1) is 1: 10～1: 15 adding distilled water by solid-liquid ratio, at 121 ℃, pressure is the 15～20min that sterilizes under the 103kPa, after the cooling, regulates initial pH to 8.0～9.0, Trichoderma viride 13030 or the mould 40505 pityrosporion ovale suspensions of healthy and free from worry wood of ratio access 2～4% by volume, the shaken cultivation temperature is respectively 30 ℃, cultivates 48h or 27 ℃, cultivates 48h or 33 ℃, cultivate 48h, rotating speed 160rpm; With the sterilization of the skin slag after the fermentation, cooling is rear to be centrifugal 10～15min under 3500～4500rpm at rotating speed, gets supernatant liquor;
(3) the supernatant liquor ratio by volume with step (2) is 1: 4 adding ethanol solution, and standing over night is centrifugal with the precipitating liquid of standing over night, abandoning supernatant, precipitation is placed 40 ℃, and vacuum is in the vacuum drying chamber of 80kPa after the vacuum drying, obtains water-soluble dietary fiber;
(4) with centrifugation gained lower sediment in the step (2), ratio by feed liquid is 1: 10～1: 15 adding distilled water, regulates pH to 10.0～11.0, suction filtration behind 70～80 ℃ of lower stirring in water bath 150min, after the filter residue vacuum drying, namely obtain insoluble diedairy fiber;
(5) collect the insoluble diedairy fiber that water-soluble dietary fiber that step (3) obtains and step (4) obtain, mix, pulverize, namely obtain dietary fiber from citrus peel residues.
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