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Patented on. 24,1946
2,413,055‘
1
' UNITED STATES‘ PATENT vOFFICE.
2,413,055’
-
raocss's roa 'rnn PREPARATION or
RIBOFLAVIN CONCENTBATES
-
Abraham Levlton, Washington, D. 0., assignor to
the United States of America, as represented by
the Secretary. of Agriculture
No Drawing. Application Mai-thee, 194s,
SerialNo. 480,951
I
‘10 Claims. (01. rev-t1)‘v
‘ ' (Granted under the act 0! March 3, 1883, as
amended April 30, 1928: 370 0. G. 757)
1
application is made under the act of
March 3, 1883, as amended by the act of April,
30, 1928,iand the invention herein described, it
patented, may be manufactured and used by or
2
.
this application to designatea product which is
intended for human consumption and which has
a ribo?avin concentration su?iciently great for
e?ective use in supplying the established mini
for the Government of the United States of
America for governmental purposes without th
mum optional requirement of ribo?avin for bread.
payment to me of any royalty thereon.
of ribo?avin for bread is 800. micrograms per- .
'
This application is a continuation-in-part of
The established minimum optional ‘requirement
pound loaf.’ Skim milk solids, when used in
my copending application i'or'patent, Serial No.
bread in normal ‘amounts, furnish only 360 mi
390,941, ?led April 29, 1941.
10 crograms per pound loaf; Based on the lactose
My invention relates to a new and useful proc
ess for the preparation of ribo?avin concentrates. .
The object of my invention is the preparation
of ribo?avin concentrates, which are character
present in the normal amount of skim milk solids
used in bread, the ribo?avin concentration nec- '
essary to satisfy the established minimum op-'
tional requirement is 80 micrograms of ribo?avin
ized by their marked potency and by their palat 15 per gram of lactose (which is to say, per gram
ability. '
'
I have found that milk sugar (lactose) as it
crystallizes will adsorb ribo?avin selectively if a.
solids). Allowing for variation in the amount of
skim solids used in bread-making, this invention
is accordingly limited to products having a riboé
?avin concentration of at least 100 micrograms
de?nite minimum concentration of ribo?avin is
exceeded, and that the adsorption of ribo?avin 20 of ribo?avin per gram‘ of lactose (or per gram
by lactose can be controlled to obtain vitamin
solids).
‘concentrates rich in ribo?avin (vitamin B2).
° My invention provides a method of preparing
vitamin concentrates comprising crystalline lac
tose and ribo?avin distributed throughout the
crystalline mass. This vitamin concentrate is
new. Neither its properties nor the manner of
preparation has hitherto been mown.
.
'
Moreover, the products of this invention being ‘
intended for human consumption, they ~are dis-'
tinguished from vitamin products intended for
animal consumptionv by their greater vitamin
concentration, by the 'palatability of any asso
ciated foreign substances, and by the compati
bility of these foreign substances with the nor
Although lactose is an important part of the
human diet, particularly of infants, it cannot 30 mal ingredients of the baking and dairy indus
tries.
\ properly be designated as a vitamin concentrate
The scope of the term “concentrate” as de?ned
even if it contains traces of ribo?avin. The term
and limited above is consistent with the gener
“concentrate”' properly designates, and is used
ally accepted standards for vitamin concentrates
throughout this application to designate, a prod
uct derived from a natural source of ribo?avin 35 used in the forti?cation and restoration of ?our
and allied substances.
' '
' '
and having a ribo?avin concentration substan
Making use of'my ?ndings concerning the ad
tially greater than the ribo?avin concentration of
the natural source.
To illustrate: Ribo?avin
sorptive properties‘ of lactose with- respect to
concentration in ‘natural products is expressed in 40 ribo?avin, I am able to prepare ribo?avin pon
terms of the number of micrograms of ribo?avin . centrates by adjusting the conditions of concen
tration and temperature of the solutionsv from
per gram solid. Whey, the liquor remaining when
which the lactose is crystallized.
‘
skim milk is treated for the removal of casein,
I have found. that at low temperatures the
as in the manufacture of casein or cheese, con
tains an average of 20 micrograms of ribo?avin 45 quantity of ribo?avin adsorbed per gram of
per gram solids. By my process ribo?avin con
.ce'ntrates can be obtained from whey having a
concentration substantially exceeding 100 micro
grams‘of ribo?avin per gram solids. Another
example is ?sh liver which contains an average
of 100 micrograms of ribo?avin per gram solids.
Ribo?avin concentrates can be prepared from
?sh liver by my process with a similar increase in
concentration.
‘
lactose is expressed by the empirical‘ formula:
4—;;'8B
(1)
where a is the quantity of ribo?avin adsorbed in
micrograms per gram of lactose; c is the initial
concentration of ribo?avin and do is the minimum
concentration of ribo?avin which mustbe ex
The term fconcentrate” is'further limited in 65 ceeded before adsorption will occur, when the
2,418,055
3
/
must be exceeded varies with the concentration -'
of alcohol, and decreases fromv 5 micrograms per
milliliter for water to 0.4 rrfcrogram per milliliter
tion of lactose and So is the concentration of
lactose'when crystallization is suspended, both
for 80 percent methyl alcohol. It also depends
upon the degree or supersaturation with respect
in grams per milliliter of water.
The application of my ?ndings can be illus-‘
trated by considering the preparation of ribo
?avin concentrates from whey. The preparation
of ribo?avin concentrates from whey is well
ad'apted'to illustrate my invention because the
to lactose, decreasing as the degree oi super
saturation with respect to lactosedecreases to a
?nal minimum value in aqueous solutions of ap
procedures are required to adjust the relative
concentrations‘ of ribo?avin and lactose. The ex
planation of these procedures provides augood
illustration oi the relation which must exist be-‘
tween theconcentrations oi ribo?avin and lactose
'in order to obtain the ribo?avin concentrates of r
this invention.
.
p
proximately 5 microgramsper milliliter of water,
10
lactose content of whey is too great to e?ect a
high unit ‘adsorption of ribo?avin by ordinary
crystallization methods. For this reason special
'
4
The minimum ribo?avin concentration which
concentration‘ of lactose is so, both in micrograms
per milliliter of water; s is the initial concentra
.
and a ?nal minimumvaluei in 80 percent methyl
alcohol of 0.4 micrograms per milliliter of 80 per
I 7 cent methyl'alcohol.
Stated in other words, there is a de?nite mini
mum concentration of ribo?avin, for any particu
lar solution, corresponding to a de?nite degree of .
supersaturation with respect to lactose which
'must be exceeded before adsorption of ribo?avin
by lactose will occur. ~ For example, if the lactose
20 concentration in a whey solution maintained at
a temperature of 5° C. is not allowed to fall be
Whey contains an average of 20 micrograms of
ribo?avin and 0.7 grams oi lactose per gram
solids.’ In the manufacture of milk sugar
low 0.72 gram per milliliter of water, adsorption
(lactose) it is customary. prior to evaporation,
gram per milliliter of water, adsorption would
occur until the ribo?avin concentration reached
5 micrograms per milliliter of water.
will not occur. v However, if the lactose concentra
tion were allowed to fall from 0.72 gram to 0.18
to remove the greater proportion of the whey
proteins and a, substantial proportion of the
mineral salts. ' The liquor (remaining after this
operation usually contains 6 percent solids of
which 80 percent is lactose, and this'liquor' can
be concentrated conveniently to 70 percent, solids.
These ?ndings make it possible to e?ect a par
, tial crystallization of lactose in a manner such
30
At 5’ C. a maximum quantity of 1.7 grams of
lactoseper milliliter of water can be crystallized
that substantially all of the ribo?avin remains
. in the mother liquor. v#I‘o illustrate: If one part
by weight of spray-dried whey powder is mixed
with 15 parts by weight oi.’ 80 percent methyl al
cohol, a solution is obtained which contains at
from the concentrated liquor- At this tempera
ture, the minimum concentration of'ribo?avin 35 room temperature 2.7 grams of excess lactose
which must be exceeded before adsorption occurs
(that is, in excess or saturation) and 133 micro
is approximately 5 micrograms permiililiter of
grams of ribo?avin per 100 grams of 80 percent
water.’ ' Inasmuch as the ribo?avin concentration
methyl alcohol. The minimum concentration of
in the concentrated, liquor is approximately 47
ribo?avin which must be exceeded before ad
micrograms per milliliter of water, the maximum 40 sorption occurs at this level of supersaturation
quantity of ribo?avin which can-be adsorbed by
with’ respect to lactose exceeds 133 micrograms
lactose is approximately 42 microgramsper milli
per 100v grams, and consequently no adsorption »
‘liter of water. This would yield a product con
occurs during theearly stages of crystallization.
taining only about 25 micrograms ‘of ribo?avin " Only when the degree of supersaturation becomes
per gram solids.
‘
-
.
a v
I have found, however, that ribo?avin concen
trates can be prepared from whey by crystallizing.
less than 0.6 gram of lactose per 100 grams of
80 percent methyl .alcohol does signi?cant ad
sorption ‘begin to take place. Corresponding to
85 percent crystallization only 3 ‘percent of the
ribo?avin is adsorbed.’ It, then, the crystalliza
the lactose in two stages, the ?rst stage being
controlled so that a‘major "portion of the lactose
crystallizes with the adsorption of only traces of 50 tion or lactose is allowed to proceed only 85 per
cent to completion, a residual mother liquor may
ribo?avin, after which the remaining lactose is
crystallized in a second stage under conditions ' be obtained following the separation of crystalline
lactose whichcontains practically all or the ribo
which result in the adsorption of substantial
?avin in solution. This liquor may then be used
quantities of ribo?avin?
.
'
As previously stated, I have found that lactose 55 as a source of ribo?avin and lactose with which
to accomplish the second stage of the crystalliza
will adsorb ribo?avin selectively if a de?nite
minimum concentration of ribo?avin is exceeded.
It follows that lactose can be crystallized ‘sub
stantially free of ribo?avin if the de?nite‘ mini
tion process.
.
>
The solids or the motherv liquor resulting from
the ?rst stage ‘of the crystallization process con
mum concentration of ribo?avin is not exceeded. 60 tain approximately 60 percent lactose. If this
liquor is subjected to distillation to recover the
Thus; when concentrated whey or spray
alcohol, a second residual liquor is obtained which
processed whey powder is mixed with methyl
can be, conveniently concentrated. The second
alcohol, the lactose as it crystallizes will adsorb
stage of the crystallization process depends on .
only traces of ribo?avin provided the ratio of
alcohol to whey solids is su?lciently great. For 65 the adjustment of the total solids concentration
of- this residual liquor within limits which will
‘example; when one part by weight of spray
now be defined. By de?nition of the term “con-l
processed whey powder is treated with not less
centrate," the lower limit of a in Formula 1 has
been set at 100 micrograms per gram of lactose.
lizes adsorbsonly traces (less than 0.1 microgram 70 The value of co and so, assuming crystallization
is to be carried substantially to completion so that
per gram) of ribo?avin. This results from the
so becomes the concentration of lactose at satu
fact that the concentration of ribo?avin in the
ration, can be determined experimentally as‘, re- .
methyl alcohol solution is less than the minimum
than 40 parts by weight of 80 percent (or less, by ‘
weight) methyl alcohol, the lactose as it crystal
> concentration which must be exceeded before ad
sorption takes place.
~
spectively, 5 micrograms and 0.18 gram per milli
75 liter of water at approximately 5° C. The value
2,413,055
5
6v
of c and s can be expressed in terms of the total
solids concentration as ‘follows:
__ % solids
c_ % solventXkl
Cheddar cheese whey was agitated with 150
pounds of 80 percent (by weight) methyl alcohol.
After agitation for several minutes, the sus
pended material was permitted to settle. The
(2) 5 supernatant liquor was syphoned off, and ?ltered,
and the residual sludge was also ?ltered. The
combined ?ltrates were stirred for approximately
?ve hours, and the lactose which crystallized was
where % solids plus % solvent equal 100%, and 10 removed by centrifugalization. 3.4 pounds of
lactose was recovered. This lactose upon analysis
hi and 102 are constants readily determinable
was found to contain 1.5 micrograms of ribo~
from analysis of the source of ribo?avin used.
‘ ?avin per gram of lactose. The ribo?avin ad
For the present consideration of the prepara
c
'
-
_ /0 sol1ds XI“
s_ % solvent
(3)
sorbed (2500 micrograms) comprised approxi;
. tion of ribo?avin concentrates from whey, For
mately 3 percent of the ribo?avin in solution, and
consequently 97 percent of the ribo?avin re
mained in the mother liquor. The alcohol was
_ % solids
‘ (4)
removed and recovered by distillation, and the
c- % water x50
residual liquor was"concentrated to contain 40
percent solids. The ‘resulting liquor was ?ltered,
% solids X0.60
s __
(5) 20 cooled to approximately 5° C., and stirred for
_ ‘7. water
several days. The lactose which crystallized was
If, then, a is set equal to 100 in Formula 1 and
separated by centrifugalization. 1.8 pounds of
Formulas 1, 4, and 5 are solved simultaneously for
lactose containing -135 micrograms ribo?avin per
mulas 2 and 3 become:
the concentration of total solids, a value of ap
proximately 55 percent is obtained. This deter
gram of. lactose was recovered comprising an
25
mines the upper limit of total solids concentra
percent. The mother liquor resulting in the last
operation could be combined with the working
tion. That is, a total solids concentration above
this limit would result in a concentrate contain
liquor in subsequent operations so that the yield
ing less than 100 micrograms of ribo?avin pe
gram of lactose.
-
The lower limit of total solids concentration
depends on solubility considerations. In order
for crystallization to occur, the total solids con
centration must be such that the concentration‘
of lactose measurably exceedsv its saturation con
centration. In the case of whey, this lower limitv
of total solids concentration is 25 percent.
If the residual whey liquor resulting from the
?rst stage of crystallization is concentrated to a
total solids concentration exceeding 25 percent 40
but not‘ in excess of 55 percent, it can/be used to
eifect a second crystallization in which adsorp
tion of ribo?avin by the crystallizing lactose will
of ribo?avin covering an extended number of
runs could be increased.
I am not ‘limited in the foregoing example to
methyl alcohol as a solvent; other solvents, such
as ethyl alcohol, acetone,‘ and isopropyl alcohol
may be used, and the proportions of alcohol and
water may be varied. It is necessary only that
the ratio between the quantity of whey solids and
the quantity of solvent be adjusted in such va
manner that the minimum concentration of
ribo?avin at which adsorption occurs is not ex
ceeded until the separation of a substantial pro
portion of the crystalline lactose has been ef
fected.
Also, it is entirely possible to effect the second
occur to the extent of not less than 100 micro
grams of ribo?avin per gram of lactose. The ac
overall yield of ribo?avin of approximately 80
Li
stage of the crystallization operation in the or
ganic solvent in which the ?rst stage was e?ected.
tual solids concentration selected within the lim
This is illustrated by the following example:
its speci?ed depends upon the vitamin concen
Example II.-10 pounds of spray-processed
tration desired. As the solids concentration ap
whey powder was stirred into 150 pounds of 80
proaches 25 percent, the degree of adsorption in
creases markedly. Quite concentrated products 50 percent (by weight) methyl alcohol. After agi~
tation for several minutes, the suspended mate
exceeding 300 micrograms of ribo?avin per gram
rial was permitted to settle. The supernatant
of lactose are obtained at solids concentrations
liquor was syphoned off and ?ltered; and the
below 30 percent.
residual sludge was also ?ltered. The combined
While the empiric relation in formula 1 above
is valid at room temperature, the temperature of LI U: ?ltrates were stirred for approximately ?ve- hours
and the lactose which separated was removed by
crystallization should be substantially below room
centrifugalization. The ?ltrate was acidi?ed
_ temperature in order to obtain a degree of en
richment consistent with good yields. I have ~ .with 150 cc. of concentrated hydrochloric acid,
and stirred. After several days, 0.45 pound of
conducted the crystallization at temperatures be
tween 5°-7° C., inasmuch as these temperatures 60 lactose containing 200 micrograms of ribo?avin
per gram of lactose had separated. These were
have been readily accessible. _ The use of lower
separated and recovered by centrifugalization.
temperatures, however, has the advantage that
The methods disclosed in Examples I and II
products of increased potency are obtained in
greater yields.
above give excellent results, but the use of or
Also, it is quite important that the crystalliza
tion be carried substantially to completion. It is
only in the later stages of the crystallization proc
’ ganic solvents involves the di?iculties inherent in
solvent recovery. I have developed an alterna
ess that substantial quantities of ribo?avin are
crystallization process which eliminates the use
of organic solvents and thus avoids these dif
adsorbed, and consequently a concentrate will
not be obtained unless crystallization proceeds
substantially to completion.
Use of this method in the preparation-of a
tive method of conducting the ?rst stage of the
?culties.
‘
I have found that the minimum concentration
of ribo?avin at which adsorption occurs is also a
function of temperature, and that it increases
the following example:
rapidly as the temperature of crystallization in
Example L-IO pounds of spray-processed 75 creases. Thus, the minimum concentration in
ribo?avin concentrate from whey is illustrated by
2,413,055
7
.
grams and the volume of water in which the
creases from a value of 5 micrograms per milli
liter oi water at 5° C. to approximately 45 micro
grams per milliliter of water at 60° C.
In my alternative method I make use or this
?nding to e?ect the crystallization of a large pro
portion of the lactose between 55° C. and 60° C.
in such a manner that practically all or the
lactose is dissolved is v milliliters, then
a’w
(i=
5 and
w
‘
s=-—
ribo?avin remains in the mother liquor. The
mother liquor is then diluted with water, cooled, 10 substituting in Formula 1
.
I)
and subjected to agitation, as a result 01 which a
a’w
second crop of lactose crystals containing the
greater portion of the ribo?avin in whey is re
covered.
7*“
T80
a= w
The concentrate obtained in this manner con
(6)
tains approximately 100 micrograms of ribo?avin 15 It has been noted previously that at approxi
per gram of lactose. The lactose corresponds in
quality to the crude lactose of commerce. The
lactose is next subjected to a re?ning operation.
mately 5° C. co and 80 are, respectively, 5 micro
grams and 0.18 gram per milliliter of water.
Formula 6 then becomes:
As a result of‘ this re?ning operation, a product
.21’
containing approximately 300 micrograms of
U
ribo?avin per gram of lactose is obtained. This
product may be re?ned further to yield an en
riched product containing more than-500 micro
grams of ribo?avin per gram of lactose.
The following example illustrates the use of
my alternative method:
Example III.--To 1000 pounds of grain curd
(7)
a:
2-0.18
1)
The application of this formula is illustrated by
considering the re?ning operation in Example
III. The crude concentrate in that example con
tained approximately 140 micrograms of ribo
?avin per gram oflactose and the refining solu
casein whey, sufficient calcium oxide was added
tion was prepared in the proportion of 30 parts
to render the acidity 0.05 percent calculated as
lactic acid. The batch was heated to boiling 30 of lactose to 100 parts of water which is substan
tially 30 grams of lactose to 100 milliliters of
(light excluded) and the supernatant liquor was
water. Thus, Formula 7 becomes:
decanted from most of_ the albuminous sludge
which formed. The liquor and then the sludge
140x30
were ?ltered and the combinedv ?ltrates were
a:
concentrated in vacuq to- contain approximately
100
30
Tad-0.18
70 percent solids. The concentrated ?ltrate was
then agitated between 55°‘ and 60° C. until
crystallization of lactose was complete. The
Solving for a, a value of approximately 330 micro
lactose crystals were separated and the resulting 40 grams of ribo?avin per gram of lactose is ob
tained as stated in Example 111. Further re?n
mother liquor which contained practically all of
ing operations may be employed to obtain an in
the ribo?avin in whey was diluted with 12 pounds
crease in purity and concentration.
of water per 100 pounds of liquor. This mixture
Also, re?ning operations may be used to ob
was cooled to, and agitated at, 5° C. until crystal
tain
a ribo?avin concentration of 'at least 100
lization was complete. The lactose, which
crystallized to the extent of 9 pounds per 1000 4 micrograms per gram of lactose from a product
containing less than that concentration. It
pounds of whey, contained approximately 140
Formula
7 is solved for the condition when a=a',
micrograms of ribo?avin per gram of lactose.
a value for a’ of approximately 28 micrograms of
This batch of lactose was dissolved in water to
ribo?avin per gram of lactose will be obtained.
yield a solution containing 30 parts of lactose 50 That is, if the re?ning operation is to lead to
per 100 parts of water. A small quantity of Filter
enrichment the concentration of ribo?avin in
Cel (?lter aid) was added (0.25 percent on the
the product to be re?ned must be at least 28
basis of lactose treated), and the mixture was
micrograms per gram of lactose. This is ex
acidi?ed with hydrochloric acid to the point at
plained by the fact that a small amount of ribo
which the acidity tested 0.09 percent. Sumcient 55 ?avin will not be adsorbed from the re?ning
calcium oxide was added to reduce this acidity
solution so that it is necessary to have an initial
to 0.05 percent. The mixture was heated to boil
concentration su?iciently high to compensate for
ing and then ?ltered. The ?ltrate was cooled to ,
°- ° C. and agitated. The lactose which crystal
this loss.
I
As a practical matter I have found it advisable,
lized contained approximately 300 micrograms of 60 in order to obtain a satisfactory rate of ,crystal
ribo?avin per gram.
The lactose was recovered
and washed with cold water. As the resulting
wash liquor contained a small amount of ribo
?avin, in large-scale operations it could be col
lected and used in processing the next batch of 65
whey.
The in?uence of the re?ning operation on the
degree of adsorption may be illustrated by ref
lization, to use a lactose concentration of at
least 0.3 grams per milliliter of water. This im
poses a further limitation on the initial concen
tration of ribo?avin, for if a in Formula 'I is set
equal to 100 and
w
is set equal to 0.3, a value for a’ of 57 micro
70 grams of ribo?avin per gram of lactose results.
erence to Formula 1:
(1:
(1)
Thus, the product to be re?ned should have at
least this concentration. Such a product can be
prepared from whey by a modi?cation of the
procedure in Example III to take advantage of
If the weight of lactose containing a’ micro
grams of ribo?avin per gram of lactose is w 75 the fact previously mentioned, that during the
9,418,055
10
crystallization process in the ?rst stage oi’ which
temperature and conditions or relative concen
tration are adjusted to allow the crystallization
of lactose substantially free of ribo?avin, and in
the second stage of which temperature and con
ditions of selective concentration are adjusted
early stages of crystallization‘ or lactose from
concentrated whey no ribo?avin is adsorbed.
The concentrations 01' ribo?avin and lactose
at which adsorption will begin at room temper
aturecan be determined from experimental re
sults to be related as follows:
to yield a ribo?avin concentrate.
I
A two-stage crystallization process is, however,
not necessary when the ribo?avin concentrate is
where s is the concentration of lactose in grams 10 prepared from a ribo?avin containing liquor de
rived from a source other than whey, because a
per milliliter of water and c is the concentration
high
initial lactose content is not encountered.
micrograms
per
milliliter
oi’
,
or ribo?avin in
It .is only necessary that such liquor be forti?ed
water. For a given value oi’ e no adsorption will
with lactose to yield a solution having relative
occur if the value of s exceeds the value de?ned
by Formula 8, and, conversely, for a given value 15 concentrations or ribo?avin and lactose such
(8) '
of s the value of 0 must be greater than that de
?nedby Formula 8 before adsorption will occur.
If, as in Example 111,.the whey ?ltrate is con
centrated to 70 percent solids, a solution is ob
tained which contains approximately 45 micro
grams of ribo?avin and 1.8 grams of lactose per
milliliter oi’ water. Solving Formula 8 for c
equal to 45 micrograms of ribo?avin, per milli
liter of water, a value for s of
(that a ribo?avin concentrate can be obtained. It
would, of course, also be possible to add sumcient
ribo?avin to whey to obtain the required condi=
- tion of relative concentration.
The conditions of relative concentration re-'
quired have been heretofore de?ned by Formula
1. The terms of Formula 1 can be rearranged as
follows:
‘
wt 0.‘? gram
of lactose per milliliter of water is obtained.
.
vThus, if the crystallized lactose is separated dur=
<9)
grams of ribo?avin per gram of lactose, so that
concentration or the solution reaches 0.7 gram
as a limiting relation Formula 9 may be stat
per milliliter, the mother liquor will retain prac
tically all of the ribo?avin originally present. 30
If the mother liquor is then cooled and crystal
lization is continued at a low temperature, the
crystallized lactose will have a ribo?avin con
centration of between 70 and 80 micrograms per
gram of lactose. If this product is subjected to
a re?ning operation, a ribo?avin concentrate can
be obtained having a concentration of approx;
imately 160 micrograms per gram of lactose.
Example 1IV.-A concentrated whey ?ltrate
containing 70 percent solids was obtained by the
-—-—a
By de?nition, a is limited to at least l00micro=
ing the crystallization process when the‘ lactose
The following example illustrates this procedure:
3
__6—6o+a8o
ed as:
'
eV
= c- 00- 10080
100
(10)
Formula 10 de?nes, in relation to’a given con
centration of ribo?avin c, the concentration of
lactose s which must not be exced if a ‘con
centrate containing at least 100 micrograms of
ribo?avin per gram of lactose is to be obtained
at temperatures substantially below room tem
440 perature.
At a temperature
becomes:
of about 5° 0. Formula 10
'
'
method set forth in Example III. This ?ltrate
was cooled to room temperature, and crystalliza
100
tion was allowed to proceed to the point at which
cc
and
So
being
5
micrograms
per milliliter of
approximately 0.7 gram of lactose per milliliter
water and 0.18 gram per milliliter of water, re
of water remained in solution. The batch was
spectively. at this temperature.
then hurriedly centrifugalized. The ?ltrate was
Concerning the purity of the ribo?avin concen=
cooled to 5°— ° C. and agitated for several days.
trates of this invention, light adsorption measure
The lactose which crystallized to the extent of
lapounds per 1000 pounds of, whey contained ap». 50 ments indicate that they are interchangeable with
admixtures of lactose and crystalline synthetic
proximately 80 micrograms of ribo?avin per
ribo?avin of like potency. Pharmaceutical prep=
gram of lactose. This batch of lactose was dis
arations of ribo?avin in tablet form usually con
solved in water to yield a solution containing 30
sist of synthetic ribo?avin admixed with the ve
parts of lactose per 100 parts oi’ water. The re
_ ?ning operation‘ from this point on paralleled 55 hicle of diluent milk sugar, and consequently my
ribo?avin concentrates may be utilized in phar
Example IE. A re?ned product containing ap
maceutical preparations directly or with supple
proximately 160 micrograms ribo?avin per gram
8___c+13
lactose was obtained.
The method used in Example IV above is, how=
ments of synthetic ribo?avin.
'
Having thus described my inventiom-I claim:
ever, not an easy one to control, because the
1. The process of preparing a ribo?avin conv
rate of crystallization of lactose is quite rapid,
which makes it rather dimcult to strike the batch
at just the proper concentration of lactose. For
this reason the method set forth in Example In
centrate which comprises forming an aqueous‘
solution of a ribo?avin-containing substance in -
I am not limited to the use of whey as a source
a proportion such that the concentration of ribo
?avin in said solution exceeds 5 micrograms per
milliliter of water, adding su?icient lactose to said
solution to obtain a concentration of lactose in
excess of 0.18 grams per milliliter of water but
not in excess of the concentration de?ned by the
of ribo?avin. Other sources, such as distilleis’
following formula
is much more easily used.
While I have illustrated my invention by the
preparation of ribo?avin concentrates from whey,
’
solubles, yeast extract, liver extract, and slops 70
from butyl alcohol fermentation processes, may
be used, lactose or whey being added to fortify
where s is the concentration of lactose which must
them with the proper proportion of lactose.
not be exceeded,v in grams per milliliter of water,
The preparation of a ribo?avin concentrate
from whey, as illustrated, entails a two-stage 75 and Q is the concentration of ribo?avin in said
I enacts"?
. . 1
11
solution, in micrograms per milliliter or water,
cooling said solution to a temperature oi’ about
5' 0., crystallising lactose from said solution
until crystallization is substantially complete, and
then recovering the crystallised .lactose, whereby 5
a ribo?avin concentrate is obtained comprising
crystalline lactose having ribo?avin adsorbed throughout the crystalline mass in the proportion >
or not less than 100 micrograms of ribo?avin per
gram of lactose.
.
p
r
'2. The process of preparing a ribo?avin con
l2
liquor until crystallisation is substantially com
plete, and then recovering said second batch of
crystallized lactose. whereby a ribo?avin concen
trate is obtained comprising crystalline lactose
having ribo?avin adsorbed throughout the crys~ '
tallinc mass in the proportion 01- not less than v
100 micrograms of ribo?avin per gram of lactose.
6. The .process or preparing a ribo?avin con
centrate from whey which comprises concentrat; '
10 ing whey to approximately '10 percent solids,
crystallizing lactose from the-concentrated whey
centrate irom whey which comprises iorming a
_ solution of whey in so percent methyl alcohol in
at a temperature of about 55' (60 60° C. until ‘
crystallisation is substantially complete, separat-.
the ratio of ‘at least 40 parts or methyl alcohol
ing the crystallized lactose, cooling the mother
per part of whey solids, crystallizing lactose from 15 liquor to a temperature of about 5° 0., crystallis
said ‘solution until crystallisation is substantially
ing a second batch or lactose irom said mother
complete, separating the crystallised lactose, re
liquor until crystallization is substantially com
moving the methyl alcohol from the mother plete, and then recoveringsaid second batch of
liquor, concentrating the mother liquor to at least
crystallized lactose, whereby a ribo?avin con
25 but not more than 55 percent solids, cooling 20 centrate is obtained comprising crystalline lactose
the mother liquor to a temperature or about 5° 0.,
having ribo?avin adsorbed throughout the crys- _
crystallizing a second batch oi lactose from the
talline mass in. the proportion of not less than
. mother liquor until crystallization is substantially
100 micrograms of ribo?avin per gram of lactose.
complete, and then recovering said second batch ' 7. The process of preparing a ribo?avin con
oi’ crystallised lactose, whereby a ribo?avin con 25 centrate from ‘whey which comprises concen
centrate is obtained comprising crystalline lactose
having ribo?avin adsorbed throughout the crys
trating whey to approximately '10 percent solids,
crystallizing lactose from the concentrated whey
talline mass in the proportion or not less than
at a temperature of about 55° to 60° C. until
crystallization is substantially complete,~separat
100 micrograms of ribo?avin per gram of lactose.
3. The vprocessor preparing a ribo?avin con 30 ing the crystallized lactose, cooling the mother
liquor substantially below room temperature, crys
centrate which comprises forming a solution of
whey in 80 percent‘ methyl alcohol in the ratio
tallizing a second batch of lactose from said
of 15 parts oi methyl alcohol per partfoi whey‘
mother liquor until crystallization is substan
, solids, crystallizing lactose from said solution for
tially complete, recovering said second batch of
approximately 5 hours, thereby crystallizing about 35 crystallized lactose. forming a supersaturated‘
85 percent of the lactose in the .said solution, ;
separating the crystallized lactose, removing the :
methyl alcohol from the mother liquor, concen '
trating the mother liquor to at least 25 but not
' more than 55 percent solids, cooling the mother 40
liquor to a temperature of about 5° 0., crystalliz
ing a second batch oi’ lactose crystals from the
mother liquor until crystallization is substantially
solution of said second batch of crystallized lac
tose in water in the proportion of at least 0.3
grams or lactose per milliliter oi water, heating
said solution to the boiling point, ?ltering said
solution, cooling the ?ltrate substantially below
room temperature, crystallizing lactose from said
filtrate until crystallization is substantially com
plete, and then recovering the crystallized lac
tose from said ?ltrate, whereby a ribo?avin con
oi crystallized lactose, whereby a ribo?avin con 45 centrate is obtained comprising crystalline lactose
having ribo?avin adsorbed throughout the crys
centrate is obtained comprising crystalline lactose
talline mass in the proportion of substantially
having ribo?avin adsorbed throughout'the crys
talline m'ass‘in the proportion of not less than ‘ more than 100 micrograms of ribo?avin per gram
of lactose. _
q
100 micrograms of ribo?avin per gram of lactose.
8. The process of preparing a ribo?avin con
4. The process of preparing a ribo?avin con
centrate from whey which comprises concentrat
7 centrate which comprises forming a solution or
whey in 80 percent methyl alcohol in the ratio ' ing whey to approximately 70 percent solids.
crystallizing lactose from the concentrated whey
or 15 parts oi’ methyl alcohol per part of whey
complete, and- then recovering said second batch ‘
_ solids, crystallizing lactose from said solution for
at a temperature of about 55° to 80" C. until
approximately 5 hours, thereby crystallizing about 55 crystallization is substantially complete, separat
ing the crystallized lactose, cooling the mother
85 percent of the lactose in said solution, sepa
liquor to a temperature of about 5° 0., crystal
rating the crystallized lactose, cooling the mother
lizing a second batch oi’ lactose from said mother
liquor‘ until crystallization is substantiallycom
ing a second batch of lactose crystals from the
mother liquor until crystallization is substantially c0 plete, recovering said second batch or crystallized
lactose-forming a solution of said second batch
complete, and then recovering said'second batch
of crystallized lactose in water in the proportion
, oi crystallized lactose, whereby a ribo?avin con
centrate is obtained comprising crystalline lac
of 30 parts of lactose to 100 parts of water, heat
tose having ribo?avin adsorbed throughout the
ing said solution to the boiling point, ?ltering said
crystalline mass in the proportion of not less than 65 solutiomcooling the ?ltrate to a temperature of
100 micrograms of ribo?avin per gram of lactose.
' about 5° 0., crystallizing lactose from said ?ltrate
' liquor to a temperature of, about 5° 0., crystalliz
5. The process of preparing a ribo?avin con
until crystallization is substantially complete, and
centrate from whey which comprises concentrat
then recovering the crystallized lactose from said
ing whey to approximately '70 percent solids, crys
?ltrate, whereby a ribo?avin concentrate is ob
tallizing lactose from the concentrated whey at 70 tained comprising crystalline lactose having ribo
' a temperature or {about 55° to 60' 0. untilcrys
?avin adsorbed throughout the crystalline mass
tallization is substantially'complete, separating . in the proportion of substantially more than 100
' the crystallizedlactose, cooling the mother liquor _ microcrams of ribo?avin per mm to lactose.
substantially below room temperature, crystalliz
9. The process of preparing a ribo?avin con
ing a second batch of lactose from said mother 75 centrate from whey which comprises concentrat
2,418,055
13
ing whey to approximately 70 percent solids,
crystallizing lactose from said concentrated whey
at room temperature until the concentration of
14
i
.
'
trating whey to approximately 70 percent solids,
crystallizing lactose from said concentrated whey’
at room temperature until the concentration of
lactose remaining‘ in solution is approximately
lactose remaining in solution is approximately
equal to the concentration de?ned by the follow 5 equal to the concentration de?ned by the follow
ing formula
ing formula
\
‘5.6
sm= 0. 80 - T
where s is the concentration of lactose remaining 10
where s is the concentration of lactose remaining
in solution in grams per milliliter of water and c
in solution in grams per milliliter of water and c
is the initial concentration of ribo?avin in micro
is the initial concentration of ribo?avin in micro
grams per milliliter of water, separating the crys
grams per milliliter‘ of water, separating the
tallized lactose, cooling the mother liquor sub
stantially below room temperature, crystallizing
crystallized lactose, cooling the mother liquor
substantially below room temperature, crystal
a second batch of lactose from said mother liquor 15 lizing a second batch of lactose from said mother
until crystallization is substantially complete, re
liquor until crystallization is substantially com
covering said second batch of crystallized lactose,
plete, recovering said second batch of crystallized
~lactose, forming a solution of said second batch
of crystallized lactose in water in the proportion
portion of at least 0.3 gram of lactose per milli
of 30 parts of lactose to 100 parts of water, heat
liter of water, heating said solution to the boiling
ing said solution to the boiling point, ?ltering
point, ?ltering said solution, cooling the ?ltrate
said solution, cooling the ?ltrate to a temperature
substantially below room temperature, crystalliz
of about 5° C., crystallizing lactose from said '
ing lactose from said ?ltrate until crystallization
?ltrate
until crystallization is substantially com~
25
is substantially complete, and then recovering the
plete, and then recovering the crystallized lactose
crystallized lactose from said ?ltrate, whereby a
from said filtrate, whereby a ribo?avin concen
ribo?avin concentrate is obtained comprising
forming a supersaturated solution of said second
batch of crystallized lactose in water in the pro
crystalline lactose having ribo?avin adsorbed
trate is obtained comprising crystalline lactose
having ribo?avin adsorbed throughout the crys
throughout the crystalline mass in the proportion
of substantially more than 100 micrograms oi’ 30 talline mass in the proportion of substantially
more than 100 micrograms of ribo?avin per gram
ribo?avin per gram of lactose.
of lactose.
10. The process of preparing a ribo?avin con
ABRAHAM LEVITON. .
centrate from. whey which comprises concen»
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