CN103404864A - Method for preparing calcium citrate malate from heads and shells of procambarus clarkii - Google Patents

Method for preparing calcium citrate malate from heads and shells of procambarus clarkii Download PDF

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Publication number
CN103404864A
CN103404864A CN2013103745115A CN201310374511A CN103404864A CN 103404864 A CN103404864 A CN 103404864A CN 2013103745115 A CN2013103745115 A CN 2013103745115A CN 201310374511 A CN201310374511 A CN 201310374511A CN 103404864 A CN103404864 A CN 103404864A
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calcium
citrate malate
calcium citrate
shrimp
head
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CN2013103745115A
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邓放明
赵玲艳
王燕
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Hunan Agricultural University
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Hunan Agricultural University
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Abstract

The invention relates to a method for preparing calcium citrate malate from heads and shells of procambarus clarkii. The method comprises the steps of preparing shrimp meal: cleaning the heads and shells of procambarus clarkii, drying the heads and shells of procambarus clarkii for 25-30 hours at the temperature of 45-55 DEG C, crushing, and sieving by using a sieve with the pore size of 60 meshes so as to prepare the shrimp meal; carrying out acid leaching: preparing mixed acid from a citric acid solution with the mass percentage concentration of 20-22% and a malic acid solution with the mass percentage concentration of 28-32% in the volume ratio of 1: (1.5-2), mixing shrimp meal (g), mixed acid (mL) and distilled water (mL) according to the ratio of 1: (3-3.5): (50-55), and leaching; and finally, carrying out ultrasonic wave assisted extraction, and carrying out vacuum drying, thereby obtaining calcium citrate malate powder. According to the method, the waste of shrimp meat processing can be utilized sufficiently during calcium citrate malate preparation, so that the preparation cost is low, and the source of raw materials is wide; the pollution to the environment caused by strong acid decalcification is avoided effectively; and the prepared calcium citrate malate has moderate calcium content and relatively high solubility.

Description

A kind of procambarus clarkia head and shrimp shell of utilizing prepares the method for calcium citrate malate for raw material
Technical field
The present invention relates to a kind of calcium-nutrition intensifying agent---calcium citrate malate, especially a kind of procambarus clarkia head and shrimp shell of utilizing prepares the method for calcium citrate malate for raw material.
Background technology
Calcium is mineral element the abundantest in human body, plays an important role in the body growth growth course.Human body self can not synthetic mineral matter, relies on extraneous supplementing and supplying with fully, and sufficient calcium is taken in and played an important role in life at human body.If human body is in status calcifames for a long time, will cause bringing out various diseases, as rickets, be the cardinal symptom of children's calcium deficiency; Adult's calcium deficiency causes skeletal calcium to reduce, and blood and intracellular calcium content increase, and cause early ageing; Pregnant woman's calcium deficiency can cause pregnancy-hypertension syndrome (preeclampsia), also can affect simultaneously the normal development of fetus; The elderly's calcium deficiency can cause osteoporosis, osteoproliferation, easy fracture, artery sclerosis, hypertension and senile dementia etc.Due to the irrationality of China's diet structure, list can not reach the purpose of replenishing the calcium from picked-up calcium natural food, is a kind of comparatively ideal approach of replenishing the calcium by the feed calcium-nutrition intensifying agent.
It is inorganic calcium hardening agent, biological calcium strengthening agent and organic calcium hardening agent that Creta Preparata in the market mainly can be divided into three types.Inorganic calcium hardening agent (ore calcium carbonate, calcium activated, chemical synthesis calcium carbonate, calcium monohydrogen phosphate, calcium phosphate, calcium chloride) is inexpensive, calcium content is high, but poorly soluble, difficulty absorbs, toxic and side effect is large; Biological calcium strengthening agent (animal bone powder biological active calcium, biological calcium carbonate, oyster shell whiting, pearl powder) is inexpensive, calcium content is higher, certain calcium-phosphorus ratio is arranged, but poorly soluble, difficulty absorbs, wholesomeness low (as remaining heavy metal, toxin); Organic calcium hardening agent (calcium lactate, calcium acetate, calcium gluconae, calcium citrate, threonic acid calcium, calcium malate, compound amino acid calcium) dissolubility is better, more easily absorbs, wholesomeness is higher.Therefore with inorganic calcium hardening agent and biological calcium strengthening agent, compare, the organic calcium hardening agent is better calcium-nutrition intensifying agent.
In the organic calcium hardening agent, calcium citrate malate (citric acid-calcium malate) has highly dissoluble, high absorbing property of biology, reduce iron absorb hinder, the characteristics such as good local flavor, safety non-toxic.In addition, compare with other calcium-nutrition intensifying agents, calcium citrate malate both had supplementing calcium element, strengthen bone density, regulate the effect such as blood fat, had again to strengthen oral health, reduce risk that kidney stone occurs, do not affect the physiological action such as other absorption of trace elements; Calcium citrate malate possesses again the physiological functions such as L MALIC ACID antifatigue, cardioprotection.Calcium citrate malate can be used as food additives, adds in bread, biscuit, cake, candy, milk powder and breakfast food and local delicacies; After can adding certain auxiliary material, directly make calcium supplement health care product, as tartaric acid Biocal, calcium citrate malate effervescent tablet; Can be used as calcium-nutrition intensifying agent adds in the beverages such as fruit juice, carrot juice, high calcium breast, soya-bean milk; Can be for the production of medicine and feed.Therefore, calcium citrate malate is current optimal calcium-supplementing preparation, has development prospect widely.
Procambius clarkii is commonly called as freshwater crayfish, in China, distributes wide, and amount of fishing is large, and the discarded object after processing accounts for the 70%-85% of raw material.But in the processing of cray at home, shrimp head and shrimp shell are except extracting shitosan, and the overwhelming majority goes out of use, and causes the wasting of resources and environmental pollution, is unfavorable for its comprehensive utilization.In these discarded objects, contain inorganic salts (being mainly the calcium salt of carbonic acid and phosphoric acid) and account for 45%.Hence one can see that, and procambarus clarkia head and shrimp shell (except eggshell) are the very good materials of exploitation calcium-nutrition intensifying agent.Therefore, utilize procambarus clarkia head and shrimp shell can greatly improve its value for raw material prepares calcium citrate malate.
Summary of the invention
Technical problem to be solved by this invention is: for above-mentioned the deficiencies in the prior art, provide a kind of method that can utilize procambarus clarkia head and shrimp shell to prepare calcium citrate malate.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of method of utilizing procambarus clarkia head and shrimp shell to prepare calcium citrate malate, and it comprises that step is:
The preparation of a, shrimp med: procambarus clarkia head and shrimp shell are cleaned, and, after 45 ℃ of-55 ℃ of dry 25-30h, pulverized, cross 60 mesh sieves, make shrimp med;
B, acidleach are carried: be that 20-22% citric acid solution and mass percent concentration are that the ratio that the 28-32% malic acid solution equals 1:1.5 ~ 2 by volume is mixed with mixed acid by mass percent concentration, by shrimp med (g): mixed acid (mL): the ratio of distilled water (mL)=1:3 ~ 3.5:50 ~ 55 is mixed, lixiviate, obtain leaching liquor;
C, ultrasonic wave assisted extraction: under the condition of ultrasonic power 200-300W, ultrasonic temperature 45-55 ℃, to the ultrasonic processing of leaching liquor obtained in the previous step 55-65min;
D, filtration, by the filtrate vacuum drying, obtain.
Further being improved to of such scheme, in step a be placed in procambarus clarkia head and shrimp shell electric drying oven with forced convection dry, and pulverize with the high speed medicinal herb grinder, makes preservation under-18 ℃ after shrimp med.
Compared with prior art, effect of the present invention has:
1, utilize procambarus clarkia head and shrimp shell to prepare calcium citrate malate for raw material, take full advantage of prawn waste, preparation cost is low, and raw material sources are wide.
2, the present invention is that 20-22% citric acid solution and mass percent concentration are that the ratio that the 28-32% malic acid solution equals 1:1.5 ~ 2 by volume is mixed with mixed acid by mass percent concentration, by shrimp med (g): mixed acid (mL): the ratio of distilled water (mL)=1:3 ~ 3.5:50 ~ 55 is mixed, lixiviate, avoided strong acid (hydrochloric acid) decalcification pollution on the environment effectively.
3, the present invention adopts the ultrasonic wave assisted extraction, makes the calcium ion recovery rate up to 94.85%, and recovery rate improves greatly.
4, by vacuum drying, to obtain outward appearance be milky crystal powder form in the present invention, and calcium content is more than or equal to 20.84%, and solubility is the calcium citrate malate that is more than or equal to 0.8015g/100mL, and the calcium citrate malate calcium content is moderate, and higher solubility is arranged.
The specific embodiment
Embodiment 1: procambarus clarkia head and shrimp shell are cleaned, and 45 ℃ of dry 30h in electric drying oven with forced convection, pulverize with the high speed medicinal herb grinder, crosses 60 mesh sieves, preserves under-18 ℃, makes shrimp med; By mass percent concentration, be that 22% citric acid solution and mass percent concentration are that the ratio that 28% malic acid solution equals 1:1.5 by volume is mixed with mixed acid, by shrimp med (g): mixed acid (mL): the ratio of distilled water (mL)=1:3.2:54 is mixed, lixiviate; Ultrasonic wave assisted extraction: under the condition of 55 ℃ of ultrasonic power 250W, ultrasonic temperature, leaching liquor is carried out to ultrasonic processing 55min, finally filter, by the filtrate vacuum drying, obtain the calcium citrate malate powder.The present embodiment calcium ion recovery rate is 94.85%, and gained calcium citrate malate powder calcium content is 20.84%, and solubility is 0.8015g/100mL.
Embodiment 2: procambarus clarkia head and shrimp shell are cleaned, at 50 ℃ of dry 28h of electric drying oven with forced convection, pulverized with the high speed medicinal herb grinder, cross 60 mesh sieves, preserve under-18 ℃, make shrimp med; By mass percent concentration, be that 20% citric acid solution and mass percent concentration are that the ratio that 30% malic acid solution equals 1:2 by volume is mixed with mixed acid, by shrimp med (g): mixed acid (mL): the ratio of distilled water (mL)=1:3:50 is mixed, lixiviate; Ultrasonic wave assisted extraction: under the condition of ultrasonic power 200W, ultrasonic temperature 50 C, leaching liquor is carried out to ultrasonic processing 60min, finally filter, by the filtrate vacuum drying, obtain the calcium citrate malate powder.The present embodiment calcium ion recovery rate is 95.12%, and gained calcium citrate malate powder calcium content is 20.86%, and solubility is 0.8215g/100mL.

Claims (3)

1. one kind is utilized procambarus clarkia head and shrimp shell for raw material, to prepare the method for calcium citrate malate, it is characterized in that comprising the steps:
The preparation of a, shrimp med: procambarus clarkia head and shrimp shell are cleaned, and, after 45 ℃ of-55 ℃ of dry 25-30h, pulverized, cross 60 mesh sieves, make shrimp med;
B, acidleach are carried: be that 20-22% citric acid solution and mass percent concentration are that the ratio that the 28-32% malic acid solution equals 1:1.5 ~ 2 by volume is mixed with mixed acid by mass percent concentration, by shrimp med (g): mixed acid (mL): the ratio of distilled water (mL)=1:3 ~ 3.5:50 ~ 55 is mixed, lixiviate, obtain leaching liquor;
C, ultrasonic wave assisted extraction: under the condition of ultrasonic power 200-300W, ultrasonic temperature 45-55 ℃, to the ultrasonic processing of leaching liquor obtained in the previous step 55-65min;
D, filtration, by the filtrate vacuum drying, obtain.
2. according to a kind of procambarus clarkia head and shrimp shell of utilizing claimed in claim 1, for raw material, prepare the method for calcium citrate malate, it is characterized in that, in step a, procambarus clarkia head and shrimp shell are placed in to the electric drying oven with forced convection drying, and pulverize with the high speed medicinal herb grinder, be equal to or less than-18 ℃ of preservations after making shrimp med.
3. according to a kind of procambarus clarkia head and shrimp shell of utilizing claimed in claim 1, for raw material, prepare the method for calcium citrate malate, it is characterized in that, in steps d, gained calcium citrate malate calcium content is more than or equal to 20.84%, and solubility is for being more than or equal to 0.8015g/100mL.
CN2013103745115A 2013-08-26 2013-08-26 Method for preparing calcium citrate malate from heads and shells of procambarus clarkii Pending CN103404864A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109907163A (en) * 2019-04-24 2019-06-21 福建省微生物研究所 Feed addictive of layer chicken and method containing calcium citrate malate are prepared using shrimp and crab shells decalcification
RU2802759C1 (en) * 2022-12-22 2023-09-01 Федеральное государственное бюджетное учреждение науки Мурманский морской биологический институт Российской академии наук (ММБИ РАН) Method for obtaining marine biological calcium from shrimp shell waste

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1775816A (en) * 2005-11-23 2006-05-24 广东海洋大学 Environment-protection low-consumption process for preparing chitin from shrimp shell and for extracting bioactivity substance
CN102050886A (en) * 2010-12-01 2011-05-11 农业部规划设计研究院 Method for producing agricultural chitosan and active calcium fertilizer by utilizing crawfish
CN102499337A (en) * 2011-10-14 2012-06-20 浙江大学 Preparation method of bioactive calcium jelly by using procambarus clarkii shells

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1775816A (en) * 2005-11-23 2006-05-24 广东海洋大学 Environment-protection low-consumption process for preparing chitin from shrimp shell and for extracting bioactivity substance
CN100398566C (en) * 2005-11-23 2008-07-02 广东海洋大学 Environment-protection low-consumption process for preparing chitin from shrimp shell and for extracting bioactivity substance
CN102050886A (en) * 2010-12-01 2011-05-11 农业部规划设计研究院 Method for producing agricultural chitosan and active calcium fertilizer by utilizing crawfish
CN102499337A (en) * 2011-10-14 2012-06-20 浙江大学 Preparation method of bioactive calcium jelly by using procambarus clarkii shells

Non-Patent Citations (1)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109907163A (en) * 2019-04-24 2019-06-21 福建省微生物研究所 Feed addictive of layer chicken and method containing calcium citrate malate are prepared using shrimp and crab shells decalcification
RU2802759C1 (en) * 2022-12-22 2023-09-01 Федеральное государственное бюджетное учреждение науки Мурманский морской биологический институт Российской академии наук (ММБИ РАН) Method for obtaining marine biological calcium from shrimp shell waste

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Application publication date: 20131127