CN105712868B - Fruits and vegetables natural organic acids calcium synthetic method using shell as calcium source - Google Patents
Fruits and vegetables natural organic acids calcium synthetic method using shell as calcium source Download PDFInfo
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- CN105712868B CN105712868B CN201610170524.4A CN201610170524A CN105712868B CN 105712868 B CN105712868 B CN 105712868B CN 201610170524 A CN201610170524 A CN 201610170524A CN 105712868 B CN105712868 B CN 105712868B
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- 150000007524 organic acids Chemical class 0.000 title claims abstract description 47
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000011575 calcium Substances 0.000 title claims abstract description 45
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 45
- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 28
- 235000005985 organic acids Nutrition 0.000 title claims abstract description 10
- 238000010189 synthetic method Methods 0.000 title claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 17
- 241000276489 Merlangius merlangus Species 0.000 claims abstract description 13
- 239000000047 product Substances 0.000 claims abstract description 13
- 235000019441 ethanol Nutrition 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000967 suction filtration Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000605 extraction Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 230000006837 decompression Effects 0.000 claims abstract description 5
- 239000000706 filtrate Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000005201 scrubbing Methods 0.000 claims abstract description 3
- 239000012141 concentrate Substances 0.000 claims description 12
- 241000237509 Patinopecten sp. Species 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 235000020637 scallop Nutrition 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- 235000009754 Vitis X bourquina Nutrition 0.000 claims description 3
- 235000012333 Vitis X labruscana Nutrition 0.000 claims description 3
- 240000006365 Vitis vinifera Species 0.000 claims description 3
- 235000014787 Vitis vinifera Nutrition 0.000 claims description 3
- 235000021028 berry Nutrition 0.000 claims description 3
- 235000020971 citrus fruits Nutrition 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 244000298715 Actinidia chinensis Species 0.000 claims description 2
- 235000009434 Actinidia chinensis Nutrition 0.000 claims description 2
- 235000009436 Actinidia deliciosa Nutrition 0.000 claims description 2
- 241000207199 Citrus Species 0.000 claims description 2
- 235000005979 Citrus limon Nutrition 0.000 claims description 2
- 244000276331 Citrus maxima Species 0.000 claims description 2
- 235000001759 Citrus maxima Nutrition 0.000 claims description 2
- 244000131522 Citrus pyriformis Species 0.000 claims description 2
- 235000007688 Lycopersicon esculentum Nutrition 0.000 claims description 2
- 241000237536 Mytilus edulis Species 0.000 claims description 2
- 240000003768 Solanum lycopersicum Species 0.000 claims description 2
- CPGKMLVTFNUAHL-UHFFFAOYSA-N [Ca].[Ca] Chemical compound [Ca].[Ca] CPGKMLVTFNUAHL-UHFFFAOYSA-N 0.000 claims description 2
- 210000004700 fetal blood Anatomy 0.000 claims description 2
- -1 lemon Chemical class 0.000 claims description 2
- 235000020638 mussel Nutrition 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 abstract description 7
- 229940093915 gynecological organic acid Drugs 0.000 abstract description 6
- 235000010323 ascorbic acid Nutrition 0.000 abstract description 4
- 239000011668 ascorbic acid Substances 0.000 abstract description 4
- 229960005070 ascorbic acid Drugs 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 2
- 229960005069 calcium Drugs 0.000 description 29
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 10
- 235000013399 edible fruits Nutrition 0.000 description 7
- 235000015170 shellfish Nutrition 0.000 description 6
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical group OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 241000237502 Ostreidae Species 0.000 description 4
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 4
- 235000015165 citric acid Nutrition 0.000 description 4
- 235000011090 malic acid Nutrition 0.000 description 4
- 239000001630 malic acid Substances 0.000 description 4
- 235000020636 oyster Nutrition 0.000 description 4
- 244000070406 Malus silvestris Species 0.000 description 3
- 239000002156 adsorbate Substances 0.000 description 3
- 235000013311 vegetables Nutrition 0.000 description 3
- 241001417490 Sillaginidae Species 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 238000005703 Whiting synthesis reaction Methods 0.000 description 2
- 235000021016 apples Nutrition 0.000 description 2
- 235000010376 calcium ascorbate Nutrition 0.000 description 2
- 229940047036 calcium ascorbate Drugs 0.000 description 2
- 239000011692 calcium ascorbate Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 229960003563 calcium carbonate Drugs 0.000 description 2
- BLORRZQTHNGFTI-ZZMNMWMASA-L calcium-L-ascorbate Chemical compound [Ca+2].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] BLORRZQTHNGFTI-ZZMNMWMASA-L 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 230000001256 tonic effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 244000144730 Amygdalus persica Species 0.000 description 1
- 244000099147 Ananas comosus Species 0.000 description 1
- 235000007119 Ananas comosus Nutrition 0.000 description 1
- 241000167854 Bourreria succulenta Species 0.000 description 1
- 206010006956 Calcium deficiency Diseases 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 241000237852 Mollusca Species 0.000 description 1
- 240000005561 Musa balbisiana Species 0.000 description 1
- 235000018290 Musa x paradisiaca Nutrition 0.000 description 1
- 244000025272 Persea americana Species 0.000 description 1
- 235000008673 Persea americana Nutrition 0.000 description 1
- 244000018633 Prunus armeniaca Species 0.000 description 1
- 235000009827 Prunus armeniaca Nutrition 0.000 description 1
- 235000006040 Prunus persica var persica Nutrition 0.000 description 1
- 244000294611 Punica granatum Species 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- 240000002547 Rosa roxburghii Species 0.000 description 1
- 235000000640 Rosa roxburghii Nutrition 0.000 description 1
- 240000007651 Rubus glaucus Species 0.000 description 1
- 235000011034 Rubus glaucus Nutrition 0.000 description 1
- 235000009122 Rubus idaeus Nutrition 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 239000004227 calcium gluconate Substances 0.000 description 1
- 229960004494 calcium gluconate Drugs 0.000 description 1
- 235000013927 calcium gluconate Nutrition 0.000 description 1
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 1
- 239000001527 calcium lactate Substances 0.000 description 1
- 229960002401 calcium lactate Drugs 0.000 description 1
- 235000011086 calcium lactate Nutrition 0.000 description 1
- 229910001576 calcium mineral Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000021022 fresh fruits Nutrition 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 208000007442 rickets Diseases 0.000 description 1
- 230000014860 sensory perception of taste Effects 0.000 description 1
- 239000003516 soil conditioner Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/185—Acids; Anhydrides, halides or salts thereof, e.g. sulfur acids, imidic, hydrazonic or hydroximic acids
- A61K31/19—Carboxylic acids, e.g. valproic acid
- A61K31/194—Carboxylic acids, e.g. valproic acid having two or more carboxyl groups, e.g. succinic, maleic or phthalic acid
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/365—Lactones
- A61K31/375—Ascorbic acid, i.e. vitamin C; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
-
- 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
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
It is an object of the invention to provide a kind of new method that fruits and vegetables natural organic acids calcium is synthesized using shell as calcium source.Main process includes shell pretreatment, the extraction of natural composite organic acid, synthesis, crystallization, washing process step.Shell is first pre-processed into obtain calcium source oyster shell whiting, chooses organic acid（Including ascorbic acid）The high fruits and vegetables of content, with 15 ~ 25% alcohol lucifuges stirring extraction 1 ~ 2 hour after scrubbing, crushing, filtering, added after filtrate decompression is concentrated in three mouthfuls of reactors of connection decompressor, separately add the distilled water of 15 ~ 20 times of volumes and excessive calcium source oyster shell whiting, pumping is depressurized, stirred, being heated to 45 ~ 60 DEG C immediately, until organic acid reacts completely, filters remove excessive calcium source oyster shell whiting while hot；After clear liquid obtained by above-mentioned suction filtration is concentrated under reduced pressure plus 95% alcohol is crystallized in 20 DEG C of refrigerator, is washed with 20 DEG C of absolute ethyl alcohols, or clear liquid obtained by above-mentioned suction filtration is freeze-dried, produces the natural composite organic acid calcium product of fruits and vegetables.Present invention process process is simple, and shell is without calcining.
Description
Technical field
The present invention relates to one kind to utilize shellfish processing waste（CONCHA MERETRICID SEU CYCLINAE, oyster shell, scallop shell etc.）For calcium source, with organic
The high fruits and vegetables of acid content are organic acid source, and process is high-valued, cleans processing step, realizes that shellfish processing waste is high-valued
The fruits and vegetables natural organic acids calcium synthetic method utilized.
Background technology
The calcium mineral matter element most as content in human body, it is not only to form the important component of bone and tooth, also exists
Played a significant role during organism physiology.Research shows that calcium deficiency can trigger a series of acalcicosises, especially to infant and
Elderly population.Therefore, rationally replenish the calcium to maintaining level of human health significant.At present, calcium tonic product main component
There are calcium carbonate, calcium gluconate, calcium lactate etc..
China is the country that shellfish culture is largest in the world, and main breed variety includes oyster, scallop, oyster, made a gift of
Shellfish etc. amounts to more than 20 and planted.Shown according to recent statistics data, only Shandong Province's shellfish culture total amount in 2015 up to 389.5 ten thousand tons, wherein
Oyster total amount is up to 85.7 ten thousand tons.Substantial amounts of shell after shellfish processing（Oyster shell accounts for more than the 80% of oyster weight）Only added on a small quantity
It is added on feed or as soil conditioner, largely goes out of use and cause serious environmental pollution.Therefore, Mollusca Resource is high-valued
Comprehensive utilization is related to the sustainable development of shellfishery, and turns into the problem of the sector is in the urgent need to address.Research hair
Existing, calcium carbonate content accounts for more than 92% in shell, can be as the calcium source of high-quality organic calcium.
Organic acid is the important component for determining fruit sense of taste in fruits and vegetables, mainly there is malic acid, citric acid, tartaric acid etc..Fruit
Vegetable kind is different, and also different citric acids are mainly distributed on citrus fruits, raspberry, grass to the type and quantity containing organic acid
In the fruits such as the certain kind of berries, pineapple, pomegranate, Rosa roxburghii；Malic acid is mainly distributed in the pip fruits such as apple, and Lee, cherry, apricot,
Citric acid and malic acid are impartial in the fruits such as peach, banana.But also there are a small number of fruit to make an exception, as grape mainly contains tartaric acid, avocado
In then lack citric acid and malic acid.Such as organic acid in fruits and vegetables is extracted and is combined into natural composite organic acid calcium with shell calcium
Salt, have the characteristics that safe to use, bioavailability is high compared with inorganic calcium.
Particular, it is important that also contain a kind of organic acid with multiple functions --- ascorbic acid in fruits and vegetables（Vc）, due to
Human body can not synthesize, and the Vc that human body needs mainly absorbs from fresh fruit of vegetables.But due to perishable rotten under fruits and vegetables normal temperature or
It is shrivelled（Vc is oxidized）And edibility is lost, thus extract natural Vc from fruits and vegetables and high natural Vc contents functional product tool is made
It is significant.In view of Vc unstability, itself and shell calcium are combined into Calcium Ascorbate, with good water solubility, stably
Property high, the features such as being rapidly absorbed by organisms and being dissociated into ascorbic acid and acceptable calcium, not only can effectively prevent and treat Vc shortages
Disease, it can also be used as the acalcicosises such as high-quality calcium tonic treatment rickets..
The content of the invention
It is an object of the invention to provide a kind of new method that fruits and vegetables natural organic acids calcium is synthesized using shell as calcium source.
To achieve these goals, main process of the invention includes shell pretreatment, the extraction of natural composite organic acid, closed
Into, crystallization, washing process step.
Shell pre-processes：Shell is removed into the adsorbates such as shell surface silt with being scrubbed after 0.05M salt acid soak 1 hour,
Wet pulverizing crosses 60 mesh sieves, then is handled through tap water flying method, 100 DEG C of drying synthesis fruits and vegetables natural organic acids calcium calcium sources
Oyster shell whiting.
Natural composite organic acid extraction：Choose the organic acids such as lemon, citrus, shaddock, Kiwi berry, grape, fresh dates, tomato
（Including ascorbic acid）The high fruits and vegetables of content are one or more of, add the distilled water of 2 ~ 4 times of fruits and vegetables weight to crush after scrubbing, with 15
~ 25% alcohol lucifuge stirring extraction 1 ~ 2 hour, filtering, volume is obtained to 1/4 ~ 1/2 times filtrate decompression concentration and be naturally compounded with
Machine acid concentrate, closed, Cord blood.
Synthesis：In in three mouthfuls of reactors of connection decompressor, natural composite organic acid concentrate and 15 ~ 20 times of bodies are added
Long-pending distilled water, the calcium source oyster shell whiting of 0.05 ~ 0.2 times of natural composite organic acid concentrate weight, immediately pumping decompression, stirring,
45 ~ 60 DEG C are heated to, until organic acid reacts completely, bubble-free effusion, filters remove excessive calcium source oyster shell whiting while hot.
Crystallization：Clear liquid obtained by above-mentioned suction filtration is concentrated under reduced pressure into 1/3 ~ 1/2 volume, adds 5 ~ 8 times of alcohol of volume 95%, in-
Crystallized in 20 DEG C of refrigerator, or clear liquid directly freezed obtained by above-mentioned suction filtration is dried, or by clear liquid obtained by above-mentioned suction filtration
It is freeze-dried after being concentrated under reduced pressure, the natural composite organic acid calcium product of solid powder fruits and vegetables can be obtained.
Washing：Crystallization is filtered out, then is washed 1 ~ 3 time with -20 DEG C of absolute ethyl alcohols, is volatilized, produces the natural composite organic acid calcium of fruits and vegetables
Product.
Present invention process process is simple, and shell is without calcining, and building-up process is without artificially adjusting reaction solution pH, products obtained therefrom
Quality is good, higher value application shell and can obtain that property is stable and the natural composite organic acid calcium of fruits and vegetables of tool multiple functions（Comprising
Calcium Ascorbate）Product.
Embodiment
Below by example, the present invention is further elaborated.
Example 1：Scrubbed after 140 grams of oyster shell is soaked 1 hour in 0.05M hydrochloric acid solutions and remove shell surface silt
Deng adsorbate, wet pulverizing crosses 60 mesh sieves, then is handled through tap water flying method, 100 DEG C of 118 grams of drying calcium source oyster shell whitings；
To select after 2 kilograms of apples are cleaned and add 4 kg of water again, crush, add 1.2 kilogram of 95% alcohol immediately, lucifuge stirs extraction 2 hours,
Filtering, concentrates filtrate to 2 liters, refilters and produce natural composite organic acid concentrate;In three mouthfuls of connection decompressor
In reactor, add 2 and die right composite organic acid concentrate and the distilled water of 20 times of volumes, 0.1 times of natural composite organic acid is dense
The calcium source oyster shell whiting of contracting liquid weight, immediately pumping are depressurized, stirred, being heated to 45 DEG C, until organic acid reacts completely, bubble-free ease
Go out, filter remove excessive calcium source oyster shell whiting while hot；Clear liquid obtained by above-mentioned suction filtration is concentrated under reduced pressure into 1/2 volume, adds 5 ~ 8 times of bodies
95% alcohol of product, is crystallized in -20 DEG C of refrigerator；Crystallization is filtered out, then is washed 1 time with -20 DEG C of absolute ethyl alcohols, volatilizes, produces fruit
102 grams of the natural composite organic acid calcium product of vegetable.
Example 2:Scrubbed after 140 grams of oyster shell is soaked 1 hour in 0.05M hydrochloric acid solutions and remove shell surface silt
Deng adsorbate, wet pulverizing crosses 60 mesh sieves, then is handled through tap water flying method, 100 DEG C of 118 grams of drying calcium source oyster shell whitings；
To select after 2 kilograms of apples are cleaned and add 4 kg of water again, crush, add 1.2 kilogram of 95% alcohol immediately, lucifuge stirs extraction 2 hours,
Filtering, concentrates filtrate to 2 liters, refilters and produce natural composite organic acid concentrate;In three mouthfuls of connection decompressor
In reactor, add 2 and die right composite organic acid concentrate and the distilled water of 20 times of volumes, 0.1 times of natural composite organic acid is dense
The calcium source oyster shell whiting of contracting liquid weight, immediately pumping are depressurized, stirred, being heated to 45 DEG C, until organic acid reacts completely, bubble-free ease
Go out, filter remove excessive calcium source oyster shell whiting while hot；It is freeze-dried i.e. after clear liquid obtained by above-mentioned suction filtration is concentrated under reduced pressure into 1/2 volume
Obtain natural 105 grams of the composite organic acid calcium product of solid powder fruits and vegetables.
Example 3：Step chooses CONCHA MERETRICID SEU CYCLINAE or scallop shell or mussel shell or conch with method with example 1 or example 2, shell
Shell, it prepares the quality of the natural composite organic acid calcium product of fruits and vegetables and oyster shell is same or like.
Claims (2)
1. using shell as the fruits and vegetables natural organic acids calcium synthetic method of calcium source, comprise the following steps：
Shell pre-processes：Shell is removed into shell surface silt and impurity absorption thing with being scrubbed after 0.05M salt acid soak 1 hour,
Wet pulverizing crosses 60 mesh sieves, then is handled through tap water flying method, 100 DEG C of drying synthesis fruits and vegetables natural organic acids calcium calcium sources
Oyster shell whiting；
Natural composite organic acid extraction：Choose the organic acid including lemon, citrus, shaddock, Kiwi berry, grape, fresh dates, tomato
One or more in the high fruits and vegetables of content, the distilled water of 2~4 times of fruits and vegetables weight is added to crush after scrubbing, with 15~25% wine
Smart lucifuge stirring extraction 1~2 hour, filtering, by filtrate decompression concentration make volume to 1/4~1/2 times natural composite organic acid
Concentrate, closed, Cord blood；
Synthesis：In in three mouthfuls of reactors of connection decompressor, natural composite organic acid concentrate and 15~20 times of volumes are added
Distilled water, the calcium source oyster shell whiting of 0.05~0.2 times of natural composite organic acid concentrate weight, immediately pumping decompression, stirring, plus
Heat, until organic acid reacts completely, bubble-free effusion, filters remove excessive calcium source oyster shell whiting while hot to 45~60 DEG C；
Crystallization：Clear liquid obtained by above-mentioned suction filtration is concentrated under reduced pressure into 1/3~1/2 volume, adds 5~8 times of alcohol of volume 95%, in-
Crystallized in 20 DEG C of refrigerator, or clear liquid directly freezed obtained by above-mentioned suction filtration is dried, or clear liquid obtained by above-mentioned suction filtration is subtracted
It is freeze-dried after pressure concentration, you can crystallized or the natural composite organic acid calcium product of solid powder fruits and vegetables；
Washing：Crystallization is filtered out, then is washed 1~3 time with -20 DEG C of absolute ethyl alcohols, is volatilized, produces the natural composite organic acid calcium production of fruits and vegetables
Product.
2. the fruits and vegetables natural organic acids calcium synthetic method using shell as calcium source as claimed in claim 1, it is characterised in that shell
For oyster shell, CONCHA MERETRICID SEU CYCLINAE, scallop shell, mussel shell, abalone shells or conch shell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610170524.4A CN105712868B (en) | 2016-03-24 | 2016-03-24 | Fruits and vegetables natural organic acids calcium synthetic method using shell as calcium source |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610170524.4A CN105712868B (en) | 2016-03-24 | 2016-03-24 | Fruits and vegetables natural organic acids calcium synthetic method using shell as calcium source |
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| Publication Number | Publication Date |
|---|---|
| CN105712868A CN105712868A (en) | 2016-06-29 |
| CN105712868B true CN105712868B (en) | 2018-03-09 |
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|---|---|---|---|
| CN201610170524.4A Expired - Fee Related CN105712868B (en) | 2016-03-24 | 2016-03-24 | Fruits and vegetables natural organic acids calcium synthetic method using shell as calcium source |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109234073A (en) * | 2018-09-28 | 2019-01-18 | 威海长青海洋科技股份有限公司 | A kind of scallop shell surface attachments scavenger and its sweep-out method |
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| CN110074417A (en) * | 2019-05-09 | 2019-08-02 | 五邑大学 | A kind of calcium tartrate agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100345502C (en) * | 2005-03-25 | 2007-10-31 | 李理 | Novel method for preparing composite organic calcium with high water solubility by using acid fruit juice and eggshell |
| KR101499292B1 (en) * | 2012-09-18 | 2015-03-09 | 주식회사 서진바이오텍 | Process for Preparing of Calcium Citrate Using Oyster Shells |
| CN103626647B (en) * | 2013-11-27 | 2015-12-02 | 青岛大学 | Take shell as the calcium type dried scallop powder synthetic method of raw material |
| CN104086395B (en) * | 2014-07-22 | 2016-07-06 | 福州大学 | The fruit acid chelating calcium product prepared with shell for raw material and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109234073A (en) * | 2018-09-28 | 2019-01-18 | 威海长青海洋科技股份有限公司 | A kind of scallop shell surface attachments scavenger and its sweep-out method |
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