This document describes a mineral feed supplement for poultry and livestock. The supplement comprises small, solid granular particles containing an intimate admixture of a normally solid wax-like material, a vegetable meal, and one or more trace minerals. This formulation protects fat-soluble vitamins from being detrimentally affected by the trace minerals when included together in feed. Examples are provided of producing various supplements using different wax and mineral sources, and testing their ability to maintain vitamin D stability over time as well as the digestibility of minerals within the formulation. The supplements were shown to greatly improve vitamin stability and mineral digestibility compared to powdered mineral mixtures.

1. * GB780022 (A)
Description: GB780022 (A) ? 1957-07-31
Improvements in or relating to feed supplements
Description of GB780022 (A)
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up-to-date or fit for specific purposes.
PATENT SPECIFICATION
780M22 Date of Application and filing Complete Specification: March
15, 1955.
No. 7593/55.
Application made in United States of America on April 2, 1954.
Complete Specification Published: July 31, 1957.
Index at acceptance:-Classes 5(2), J(2; 3C); 49, BIC; and 81(1), B(3;
4: 6).
International Classification:-A23d, k. A61k.
COMPLETE SPECIFICATION
Improvements in or relating to Feed Supplements We, Nopco CHEMICAL
COMPANY, a Corporation duly authorised and existing under and by
virtue of the Laws of the State of New Jersey, United States of
America, of First and Essex Streets, Harrison, New Jersey, United
States of America, do hereby declare the invention, for which we pray
that a patent may be granted to us, and the method by which it is to
be performed, to be particularly described in and by the following
statement:-
This invention relates to supplements of socalled trace minerals which
are suitable for addition to fat-soluble vitamin-containing
supplements for poultry and livestock feeds.
It is common practice in the poultry and livestock feed field to add

2. various minerals to poultry and livestock feeds. For example many such
feeds have mineral supplements added to them which are mixtures of
materials such as limestone, steamed bone meal, dicalcium phosphate
and salt. Such mineral materials are added to poultry and livestock
feeds in amounts which are comparatively large as compared to the
amounts of so-called trace minerals which are added to such feeds. The
trace minerals most frequently added to feeds are compounds of
manganese, copper, iron, cobalt and iodine. Supplementary amounts of
these trace minerals are usually considered to be necessary for swine
and cattle, and all of them, with the exception of cobalt, are
considered to be necessary additions for poultry feeds.
It is also common practice to supplement poultry and livestock feeds
with fat-soluble vitamins and particularly with vitamins A and D. In
many cases feed manufacturers desire to purchase supplements for
addition to their feeds which supplements contain both fatsoluble
vitamins and minerals, and this is particularly true as far as the
trace minerals are concerned.
Most minerals have a very detrimental effect on vitamins A and D and
other fat-soluble vitamins such as vitamin E particularly in the types
of vitamin and mineral supplements which the feed manufacturers desire
to use [Price 3s. 6d.] fice 42 e since in such supplements the
concentration of the minerals is of course considerably higher than in
the finished feed product. The trace minerals are particularly
destructive of the fatsoluble vitamins, especially vitamin D.
Vitamin A is quite susceptible to destruction by oxidation even if
minerals are not present though minerals do accelerate the oxidation
of vitamin A and, as pointed out above, vitamin D is quite susceptible
to destruction when exposed to various minerals. Many attempts have
been made in the past to prepare fat-soluble vitamin products which
are resistant to oxidative destruction but in most cases such attempts
have not been too successful. For instance fat-soluble vitamin
supplements which are very resistant to destruction by the oxidising
influences of the atmosphere have been prepared by admixing at
elevated temperatures a fat-soluble vitamin-containing material, a
normally solid wax-like material having a melting point of at least
about 450 C., an edible antioxidant, and a vegetable flour. This
mixture is then formed into a multiplicity of small, solid spheroidal
particles. The fat-soluble vitamins in these products are extremely
resistant to the oxidising influences of the atmosphere and are
extremely resistant to the destructive action of most mineral
mixtures. It has been found, however, that the vitamin D in such
products is sometimes detrimentally affected by the trace minerals
particularly when the trace minerals are present with the vitamin
Dcontaining products in a relatively high concentration.

3. It is the object of this invention to provide trace minerals in a form
in which they will be readily digestible by poultry and by livestock
but will not detrimentally affect the stability of any fat-soluble
vitamins with which they may be associated.
According to the present invention a mineral feed supplement comprises
a multiplicity of small, solid granular particles, the majority of
such particles being of a size such that they will pass through a 16
mesh screen but will be retained on a 60 mesh screen, each solid
9/i.+Q as particle being an intimate admixture of (1) a normally solid
wax-like material having a melting point of at least 98 F. (37' C.),
(2) a vegetable meal and (3) a trace mineral or trace minerals
considered necessary for normal nutrition.
The screen sizes specified herein refer to the United States Standard
Sieve Series.
The term " normally solid wax-like material" is used herein to connote
glycerides, other fatty acid esters, free fatty acids, vegetable
waxes, mineral waxes and similar materials or mixtures of such
materials which have a melting point of 98 F. (370 C.) or above. Among
such materials are hydrogenated fats and oils such as hydrogenated
coconut oil, hydrogenated cottonseed oil, hydrogenated peanut oil,
hydrogenated soyabean oil and hydrogenated fish oils, fatty acids such
as stearic acid; mineral waxes such as the various petroleum waxes,
vegetable waxes such as carnauba wax, candelilla wax, ouricury wax;
and animal waxes such as beeswax.
Among the vegetable meals which can be employed are soyabean meal,
maize germ meal, cottonseed meal, linseed meal, wheat germ meal, maize
meal, alfalfa leaf meal, wheat bran, rice bran, oatmeal and peanut
meal. Preferably the majority of the particles of the vegetable meal
used should pass through a 20 mesh screen.
Any trace mineral which it is desired to incorporate in the finished
poultry or livestock feed may be used in preparing the products of the
invention. As pointed out above, the most common trace minerals which
are added to such feeds are compounds of manganese, copper, iron,
cobalt and iodine.
In preparing the products of the invention, the normally solid waxlike
material which is to be used is heated until it is in a completely
liauid state. Thereafter the trace mineral or minerals and the
vegetable meal are added to the wax-like material with efficient
stirring in order to get a uniform mixture of the minerals in the
product. The trace minerals are added to the normally solid wax-like
material prior to the addition of the vegetable meal although, if
desired, the order of addition can be reversed. After thorough mixing
of the ingredients has been completed, the product is allowed to cool
slowly while efficient stirring is continued. The product which is

4. obtained is a granular meal free from dustiness with a majority of the
Darticles passing through a 16 mesh screen and being retained on a 60
mesh screen.
The relative proportions of the three ingredients of the product can
vary somewhat. Preferablv the trace minerals make up from 300,% to
700% by weight of the product, the normally solid wax-like material
preferably makes up from 10% to 20% by weight of the product and the
vegetable meal preferably makes up from 20, to 50%A by wreight of the
product.
Trace mineral supplements prepared in the above manner are readily
digestible yet the trace minerals contained therein have very much
less destructive action on fat-soluble vitamins.
Certain specific examples (Examples II-X) will now be described by way
of illustration as to how the invention may be performed, preceded by
an example (Example I) of a known trace mineral mixture for
comparison. In the examples all parts are expressed by weight.
EXAMPLE I.
A trace mineral mixture of the type commonly employed for adding such
minerals to poultry and animal feeds was prepared by mixing together:
Managanous oxide 61.98 parts Cupric hydroxide 2.236 Red iron oxide
34.19,, Stabilised potassium iodide (90%;. potassium iodide and 10%
calcium stearate) 1.278 Cobalt carbonate 0.3195,, The resulting
mixture was a very fine powder.
This product represents the usual types of trace mineral mixtures used
in adding such minerals to poultry and animal feeds and does not
embody the present invention.
EXAMPLE II.
A product embodying the present invention 95 was prepared by melting
8.5 parts of microcrystalline wax having a melting point of 1700 F.
(77 C.) and then adding to the melted wax parts of the product of
Example I and thoroughly mixing these two ingredients with 100
efficient stirring and thereafter, while this mixture was kept above
170 F. (77 C.), 16 parts of soyabean meal were added thereto with
efficient stirring. Thereafter the mixture of the three ingredients
was removed from the source 105 of heat and allowed to cool slowly
while stirring of the mixture was continued. The resulting product
embodying the invention was a granular meal which was free of
dustiness and the majority of the particles of which passed 110
through a 16 mesh screen but were retained on a 60 mesh screen.
EXAMPLE III.
Another product embodying the invention was prepared in the same
manner as the product of Example II except that the microcrystalline
wax which was employed had a melting point of 190 F. (880C.).
EXAMPLE IV

5. Another product embodying the invention was prepared in the same
manner as in Example II except that the microcrystalline wax was
replaced by completely hydrogenated soyabean oil.
EXAMPLE V.
Still another product embodying the inven780,022 38.2 g. of a calcium
pantothenate premix containing 12.5% d-calcium pantothenate in a
carrier of solvent-extracted rice bran meal 1540 g. of a choline
chloride premix containing 25% choline chloride on a carrier of corn
distiller's dried grains 4.13 g. of 80% procaine penicillin on a
carrier of Fuller's Earth 187.5 g. of a crude fermentation product
containing 16 mg. of vitamin By, per pound 2370 g. of
solvent-extracted rice bran meal.
Each of the products of Examples I to IV was combined with a portion
of the vitaminantibiotic premix and with a Vitamin D, product by
admixing at elevated temperature a material containing Vitamin D,, a
normally solid wax-like material having a melting point of at least
450 C., an edible antioxidant, and a vegetable flour, and forming the
mixture into a multiplicity of small, solid spheroidal particles. This
vitamin D. product was guaranteed to contain 15,000 I.C.
(International Chick) units of vitamin D, per gram. The actual vitamin
D, content of this product was in excess of this amount by 30% since
it is the custom of manufacturers to supply approximately this excess
of vitamin D, in such products. The five compositions prepared in this
manner, labelled "Product A" to " Product E," contained the following
proportions by weight of the materials shown:
tion was prepared as in Example II except that the microcrystalline
wax was replaced with crude scale wax (a crude paraffin wax).
EXAMPLE VI.
In this Example the effect of the mineral mixtures of Examples I to V
inclusive, on the stability of fat-soluble vitamins was determined by
preparing vitamin-mineral supplements in the form in which they would
be used by the commercial feed manufacturer and then testing the
stability of the vitamin D, in such vitamin-mineral mixtures under
rigorous test conditions.
In carrying out this test a vitamin-antibiotic premix was prepared
containing the following:
146 g. of a vitamin A-containing product prepared by admixing at
elevated temperature a material containing Vitamin A, a normally solid
wax-like material having a melting point of at least 450 C., an edible
antioxidant (butylated hydroxy anisole with lecithin as a synergist),
and a vegetable flour, and forming the mixture into a multiplicity of
small solid spheroidal particles which contained 10,000 U.S.P. (United
States Pharmacopoeia) units of vitamin A per gram 26.25 g. of a
riboflavin premix containing grams of riboflavin per pound in a

6. soyabean meal carrier 79.3 g. of a premix containing 25% niacin in a
carrier of solvent-extracted rice bran meal Ingredient Product Product
Product Product Product Multivitamin antibiotic premix Vitamin D3
product Mineral product of Example I
Mineral product of Example II
Mineral product of Example III Mineral product of Example IV
A B 175.7 175.7 4.42 C D E 175.7 175.7 175.7 4.42 4.42 4.42 4.42 6.15
- 10.46 -- 10.46 - - - 10.46 Mineral product of Example V
Solvent-extracted rice bran meal - 10.46 13.55 9.24 9.24 9.24 9.24 The
only essential difference between these five mixtures was the fact
that the trace minerals in Product A were in their original powdered
form whereas those present in Products B, C, D and E were the mineral
supplements embodying the invention. All five products contained the
same amounts of the trace minerals.
The five products were all prepared to contain 150,000 I.C. units of
vitamin D, per 90 pound based upon the guarantee for the vitamin D,
product. Samples of all five were stored 60780,022 at 98' F. (37 C.)
and portions were removed for vitamin D assay after 11 months and 3
months at this temperature. The assays were conducted biologically
employing the rat, according to the U.S.P. Procedure. The results are
summarized in the table below:
Vitamin D, found, I.C. Units per pound After 1- Months After 3 Months
at 98'F (373C) at 980F (370C) Product A Product B Product C Product D
Product E Very much less than 150,000 150,000 150,000 150,000 150,000
150,000 150,000 150,000 150,000 These data illustrate the greatly
improved stability of vitamin D, in the multivitaminantibiotic trace
mineral mixes due to the treatment of the finely divided trace
minerals in accordance with the invention. In the case of Product A
after storage for 11 months at 98' F. (37 C.), the biological assay
showed an average healing of 1.5 as compared with a healing of 4.8 for
a group of rats receiving the theoretical dosage of vitamin D
equivalent to the amount that should have been present if no
destruction of vitamin D had occurred in Product A. This indicates a
loss of a considerable portion of the vitamin D present originally and
in fact that product could not have contained more than 75,000 I.C.
units per pound at the end of the 1. months storage period.
EXAMPLE VII.
In order to test the digestibility of the mineral supplements
embodying the invention, a tracer technique was employed. Two
watersoluble vitamins, thiamine and riboflavin, were employed as the
tracers. These were finely divided powders which were mixed with the
trace minerals prior to incorporating the minerals in a product
embodying the invention.
The mineral supplement containing these two vitamins was then

7. administered orally in gelatine capsules to five human subjects and
the urinary excretion of thiamine and riboflavin measured and compared
with the excretion obtained after dosage with equivalent amounts of
the two vitamins taken in unprotected form in the same manner. This
technique for measuring digestibility has been used in a considerable
number of similar applications and has been described in the chemical
literature (see "Physiological Availability of the Vitamins i by Oser,
Melnick and Hochberg, Analytical Edition, Industrial and Engineering
55 Chemistry, Vol. 17, page 405, July 15, 1945).
The details of the test are described below:
The following composition was prepared:
Ingredients Product of Example I 35.00 g.
Microcrystalline wax (m.p. 1 b0, F.). 10.67, Soyabean oil meal 16.00,,
Riboflavin 4.47,, Thiamine hydrochloride 4.47,, Process The wax was
melted and the minerals and vitamins added with stirring. While the
mixture was kept hot, the soyabean meal was incorporated and the total
blend allowed to cool with stirring. The final product was similar in
appearance to the products of Examples II to V. It contained
additional wax so that the ratio of the total amount of wax to the sum
of the minerals and vitamins was the same as in the products of
Examples II to V.
Each human subject in the biological assay ingested 0.1457 g. of this
product containing mg. of thiamine hydrochloride and 10 mg.
of riboflavin.
The principle of this biological assay is based upon the fact that
normal human subjects, free of vitamin deficiencies, and ingesting a
standardized diet, excrete a certain normal low level of the
water-soluble vitamins in their urine.
When an additional dose of the vitamin is fed in a standardized
manner, a certain relatively fixed fraction of the additional dose is
also excreted in the urine during the subsequent 24 hour period. In
the digestibility tests described here, the normal daily excretion
without extra vitamins is established. This is called the basal. The
24 hour excretion is also determined after the administration 10 mg.
of thiamine and 10 mg. of riboflavin mixed with soya flour and placed
in a readily soluble gelatine capsule.
Finally the excretion is measured following the administration of an
equivalent amount of the two vitamins in the form of a product whose
digestibility is to be determined. The urinary excretion of the five
subjects used in this investigation under each of these three
conditions is summarized in the table below:
780,022 7so80,622 URINARY EXCRETION OF WATER-SOLUBLE VITAMINS, MG. PER
24 HRS.
THIAMINE Subject Basal After ingesting vitamins in soya flour After

8. ingesting vitamins in product of present invention 1 0.20 1.08 1.77 2
0.16 0.66 1.63 3 0.22 1.01 0.97 4 0.22 1.63 1.23 0.27 1.06 1.27
Average 0.22 1.09 1.37 RIBOFLAVIN After ingesting After ingesting
vitamins in soya vitamins in product Subject Basal flour of present
invention 1 1.17 6.00 7.05 2 0.78 5.20 6.97 3 1.01 5.56 3.84 4 0.67
5.36 5.10 0.96 5.56 5.79 Average 0.92 5.54 5.75 The degree of
availability can be calculated for each vitamin separately by
subtracting the basal excretion from that obtained after each test
dose, and then dividing the difference for the treated vitamins by the
difference for the untreated vitamins and multiplying by 100 as
illustrated below:
1.09 - 0.22=0.87 1.37 - 0.22 1.15 1.15 - x 100= 132% availability of
thiamine 0.87 5.54 - 0.92=4.62 5.75 - 0.92 = 4.83 4.83 - x 100=105%
availability of riboflavin 4.62 These calculations show a vitamin
availability of 132% for thiamine and 105% for riboflavin. In the case
of thiamine, it is not uncommon to find between 120 and 140%
availability when testing coated vitamins since the coating appears to
exert a protective effect in the gastro-intestinal tract.
It is well recognized that the digestive tracts of poultry and
livestock are more efficient than the digestive tract of man.
Therefore since the products embodying the invention contain the
minerals in a form completely available to man, the minerals in such
products are also completely available to poultry and livestock.
EXAMPLE VIII.
Another product embodying the invention was prepared in the same
manner as the product of Example II except that the soyabean meal was
thoroughly admixed with the heated microcrystalline wax and thereafter
the trace minerals were added to the liquid mixture of the wax and the
soyabean meal.
EXAMPLE IX.
The product of Example VIII was shown to be very effective for adding
trace minerals to vitamin supplements by mixing that product with a
multivitamin-antibiotic mixture similar to that described in Example
VI except that vitamninD2 was substituted for the vitamin D, used in
Example VI and except that chlortetracycline hydrochloride was
substituted for procaine penicillin. Also the level of fortification
of this mix with vitamin D2 was at a guaranteed level of 300,000
U.S.P. units of vitamin D, per pound with an actual level of 375,000
U.S.P. units of vitamin D, per pound.
The levels of other vitamins in this mix also differed somewhat from
that of Example VI.
A comparable stability test was carried out on two
multivitamin-antibiotic-trace mineral mixtures prepared in this manner
using in one case as the source of trace minerals the product

9. embodying the invention referred to in Example VIII and in the other
case the standard trace mineal mixture of Example I. After storage for
one month at 98 F. (370 C.) the product prepared using the trace
mineral mixture of Example I showed no antirachitic activity whatever
for rats at a testing level ot 300,000 U.S.P. units per pound. This
means that the product after one month storage could not contain any
more than one-fourth of its intended potency of 300,000 units per
pound.
The product prepared using the mineral mixture embodying the invention
as illustrated in Example VIII was stored for three months at 98 F.
(370 C.). The potency of the product was tested at a level of 300,000
units per pound at the end of 12 months and at the end of the 3 month
period. In both cases it was found that the product prepared using the
mineral mixture of Example VIII contained the guaranteed 300,000 units
per pound. It is apparent that the stabilized mineral mixtures
embodying the invention have very greatly improved compatibility with
fat-soluble vitamins even under very rigorous conditions.
In this example and in Example VI the stability of vitamin A was not
determined since it is well recognised that vitamin D. and vitamin D,
are much more sensitive to destruction by trace minerals than is
vitamin A.
EXAMPLE X.
A product embodying the invention was prepared in the same manner as
the product of Example II except that the microcrystalline wax was
replaced with beeswax and the amounts of the three ingredients used
were 5 parts of beeswax, 15 parts of the product of Example I and 10
parts of soyabean meal. The resulting product was very similar in
appearance to the products of Examples II to V and Example VIII and
had the same excellent characteristics as those products.
In addition to being highly useful for adding trace minerals to
fat-soluble vitamincontaining materials, the products of the invention
are highly useful for adding trace minerals to any feed or other
material which contains a fatty material. It is well known that trace
minerals normally have a tendency to catalyze the development of
rancidity in fatty materials. However such is not the case with the
products of the invention.
Although the products of the invention find their biggest use in
adding trace minerals to poultry and livestock feeds, they are also
highly useful for adding trace minerals to pharmaceutical products and
to human foods, particularly if such products or foods contain any
fatsoluble vitamins or any fatty material subject to rancidity.
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