Food or edible material: processes – compositions – and products – Product with added vitamin or derivative thereof for...
Reexamination Certificate
2000-10-12
2001-11-20
Sayala, Chhaya D. (Department: 1761)
Food or edible material: processes, compositions, and products
Product with added vitamin or derivative thereof for...
C426S074000, C426S656000, C426S807000
Reexamination Certificate
active
06319528
ABSTRACT:
CROSS-REFERENCE TO RELATED APPLICATION
This application is based on German Application Nos. DE 199 20 507.8, filed May 5, 1999 and DE 100 16 321.1, filed Mar. 31, 2000, which disclosures are incorporated herein by reference.
FIELD OF THE INVENTION
The invention relates to an animal feedstuff additive based on a fermentation broth, which contains D-pantothenic acid and/or one or more of its salts and a process for preparing this additive.
BACKGROUND OF THE INVENTION
Pantothenic acid is produced all over the world on a scale of several thousand tonnes per year. A large part of the pantothenic acid produced is used for feeding economically useful animals such as poultry and pigs. Demand is increasing.
Pantothenic acid may be prepared by chemical synthesis or biotechnically by the fermentation of suitable microorganisms in suitable nutrient solutions. In the case of chemical synthesis, DL-pantolactone is an important precursor. It is prepared in a multi-stage process from formaldehyde, isobutylaldehyde and cyanide. In further process steps, the racemic mixture is separated and D-pantolactone is condensed with &bgr;-alanine, thus producing D-pantothenic acid.
The typical commercial form is the calcium salt of D-pantothenic acid. The calcium salt of the racemic mixture of D,L-pantothenic acid can also be used.
The advantage of fermentative preparation using microorganisms is the direct formation of the desired stereoisomeric form, that is the D-form, which contains no L-pantothenic acid.
Various types of bacteria such as, for example,
Escherichia coli, Arthrobacter urea faciens, Corynebacterium erythrogenes, Brevibacterium ammoniagenes
and also yeasts such as, for example,
Debaromyces castellii
may, as shown in EP-A-0 493 060, EP-A-0 590 857 and WO 97/10340, produce D-pantothenic acid under suitable conditions of fermentation. Particularly suitable microorganisms are the derivatives of
Escherichia coli
IFO3547 described therein, such as e.g. the strains FV5069/pFV31 or FV5069/pFV202.
During the fermentative preparation of D-pantothenic acid, as described in EP-A-0 493 060, EP-A-0 590 857 and WO 97/10340, a microorganism capable of D-pantothenic acid production is cultivated in a suitable nutrient and the D-pantothenic acid produced is then isolated in a costly manner, purified and prepared as the calcium salt.
Suitable nutrient media contain a source of carbon such as e.g. glucose or starch flour hydrolyzate or sucrose or molasses, precursors such as e.g. &bgr;-alanine,D,L-pantoic acid or D,L-pantolactone, a source of nitrogen such as e.g. ammonium sulfate, a source of phosphorus such as e.g. potassium phosphate and other salts, trace elements and vitamins and optionally complex media additives such as e.g. yeast extract. The microorganisms are then incubated in this medium at a suitable pH, with appropriate aeration and stirring, wherein these then excrete D-pantothenic acid.
According to the current prior art, which is represented by WO96/33283 and EP-A-0 590857, the calcium salt of D-pantothenic acid is obtained from the pantothenic acid-containing fermentation broth by costly isolation and purification. After initial isolation of the biomass by filtering or centrifuging, further processing of the filtrate is performed by purification using active carbon or column chromatography. After reaction of the solutions obtained in this way with calcium hydroxide, the desired Ca salt crystallizes out.
According to WO 96/33283 the filtrate is decolored with active carbon in the first column. The pH is adjusted to 3.0 with concentrated hydrochloric acid and the liquid is then continuously purified over two further columns packed with active carbon. Elution of the D-pantothenic acid is achieved with the aid of methyl alcohol. After the subsequent neutralization step using Ca(OH)
2
powder, a solution is obtained from which calcium D-pantothenate is recovered by crystallization at 5° C.
In the method described in EP-A-0 590 857, the filtrate is first purified with the aid of cation and anion exchanger columns. Elution is performed with hydrochloric acid. The eluted fraction is then neutralized with Ca(OH)
2
, active carbon is added thereto and the mixture is filtered. The filtrate obtained is then extracted into a low molecular weight alcohol (methanol, ethanol, isopropanol) and calcium D-pantothenate is obtained by crystallization.
The calcium D-pantothenate prepared in the way described above is used as an additive in feedstuff for animal nutrition.
SUMMARY OF THE INVENTION
According to the prior art, salts of D-pantothenic acid and D,L-pantothenic acid are prepared by reacting the acid, prepared by chemical synthesis or fermentation, with the desired salt solutions.
The object of the invention is to provide new preparative forms of D-pantothenic acid and its salts which are suitable as feedstuff additives.
Furthermore, an object of the invention is to provide a method of preparation which is more economical and more efficient than the currently known processes.
The invention provides an animal feedstuff additive based on a fermentation broth, characterized in that it contains p
1
a) D-pantothenic acid and/or its salts, in particular alkali metal or alkaline earth metal salts, p
1
b) the biomass formed during fermentation in an amount of 0 to 100% and p
1
c) at least the greater part of the other dissolved ingredients of the fermentation broth and p
1
d) is present in solid form, in particular in a finely divided or granulated and free-flowing form.
Depending on the requirements, the animal feedstuff additives are generally provided as spray dried or freeze-dried, finely divided, free-flowing powders, or else in granulated form, which may contain different proportions of biomass. The bulk density is in particular about 500 kg/m
3
. The additives are storage-stable.
If the biomass is isolated, naturally other solids, for example inorganic solids, are also removed. In addition, the additive according to the invention contains at least the greater part of the other substances produced or any added substances which are present dissolved in the fermentation broth, provided they have not been separated by suitable processes.
These substances may include organic secondary products which are produced and excreted by the microorganisms used during fermentation, in addition to D-pantothenic acid. These include L-amino acids chosen from the group L-methionine, L-lysine, L-valine, L-threonine, L-alanine or L-tryptophane, in particular L-valine. Furthermore, organic acids which contain up to three carboxyl groups such as e.g. acetic acid, lactic acid, citric acid, malic acid or fumaric acid are also included. Finally, sugars which are poorly convertible, such as e.g. trehalose, are also included. These compounds are optionally desirable if they contribute to the value of the additive.
Furthermore these substances may include groupings from the convertible sugars used such as e.g. glucose or saccharose.
The invention also provides a process for preparing a feedstuff additive which contains D-pantothenic acid and/or its salts, which is characterized in that p
1
a) the D-pantothenic acid-containing broth which generally contains sodium, potassium, ammonium, magnesium or calcium salts is prepared by fermentation, p
1
b) the biomass is optionally completely or partly separated from this, p
1
c) the hydroxide or oxide of an alkaline earth or alkali metal is added to the solution or broth obtained in this way, preferably in stoichiometric amounts with respect to the D-pantothenic acid, and p
1
d) the mixture obtained in this way is dried, spray dried, spray granulated or granulated.
The invention also provides a process for preparing feedstuff additives which contain D-pantothenic acid and/or its sodium, potassium, ammonium, magnesium or calcium salts in the range from 20 to 80 wt. % (dry weight) from fermentation broths, characterized by the steps p
1
a) preferably, removal of water from the fermentation broth (concentration step), p
1
b) optionally, removal of 0 to 100% of the biomass formed
Becker Ulrich
Binder Michael
Friedrich Heinz
Pfefferle Walter
Uffmann Klaus-Erich
Degussa - Aktiengesellschaft
Pillsbury & Winthrop LLP
Sayala Chhaya D.
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