May 20, 1958

METHOD OF PRODUCING CURED WANIE

GJENTIO IVNTVA
ONV/ BWAZNE

N.398) ·NV/38 E
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INVENTORS

ATTORNEYS
 United States Patent Office
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2,835,591
Patented May 20, 1958
1. 2
are not developed until the curing step, and undesirable
2,835,591 loss of such properties is eliminated.
METHOD OF PRODUCING CURED WANLLA EX With the above in mind, the primary object of this
TRACT FROM GREEN VANILLABEANS invention is to produce cured vanilla extract from green
vanilla beans by a process which results in retention of
Robert Edwin Graves and Richard Leland Hall, Balti vanilla flavor and odor to a far greater degree than was
more, and Albert Joseph Karas, Caton Esville, Md., as achieved by processes heretofore employed.
signors to McCormick
Md., a corporation & Company, Inc., Baltimore,
of Maryland Another object of this invention is to provide a proc
eSS for producing cured vanilla extract from green vanilla
10 beans whereby substantially all of the constituents which
Application August 23, 1955, Serial No. 530,052 impart characteristic favor to vanilla and contribute to
24 Chaims. (C. 99-140) the characteristic aroma of vanilla, are retained in the
final extract.
The present invention relates to a new method for pro 15 Aforfurther object of this invention is to provide a proc
ducing cured vanilla extract from green vanilla beans. ess producing cured vanilla extract from green vanilla
beans which comprises extracting green bean extract from
More particularly, our invention relates to the curing green vanilla beans in the absence of oxygen, concentrat
of green vanilla bean extract after extraction thereof ing. Such extract under a vacuum, then curing the con
from the
thereof.
mature green.
vanilla .
bean and concentration
- centrated extract and adding ethyl alcohol to thereby
20 produce a cured vanilla extract.
it should immediately be noted that the invention rep Still another object of this invention is to provide a
resents a novel and radical departure from former proc novel
esses, because extraction and concentration of green bean extract process to
for curing a concentrated vanilla bean
thereby form cured vanilla extract without
extract are initially carried out followed by curing of the destroying the constituents which impart characteristic
green bean extract in that form. Such process prevents 25 flavor to the vanilla and contribute to the characteristic
the destruction and dissipation of the natural volatile oils aroma of vanilla.
and other constituents which contribute the aroma and Another and more specific object of this invention
flavor characteristics of vanilla. Thus, a final vanilla is to provide a novel process for producing cured vanilla
Xtract is obtained of far richer flavor and aroma than
realized by prior processes wherein curing preceded ex 30 extract from green vanilla beans as noted heretofore,
wherein one or more enzymes may be added to the
traction and concentration.
Various methods have been utilized in the past for ing, vanilla
thebeans
curingorprocess.
bean extract at any point prior to, or dur
the preparation of cured vanilla extract from vanilla
beans. In this respect, it should immediately be noted in Other part
and further objects of the invention will be
apparent and in part set out in the detailed de
that the unripe, or green vanilla bean has no vanilla 35 scription of the several steps in the process which follows.
favor or odor and these are developed during a curing Referring to the accompanying drawing, we illustrate
process.
Curing has previously been performed by various proc a flow diagram of the various steps comprising the proc
?SS.
esses. Naturally, vanilla beans will cure if left on the In step I, a given weight of mature green vanilla
vine and this is, of course, the earliest known means of 40 beans of a known moisture content are finely chopped
accomplishing such curing. Later on, this primitive in an oxygen-free atmosphere. A typical moisture con
method of curing was improved upon through the use tent of the bean is about 85%. Any conventional chop
of processes such as the Mexican and Bourbon processes. ping means can be utilized.
In the Mexican process, the green beans are placed on Step II contemplates extracting the green bean ex
blankets and are exposed to the direct rays of the sun 45 tract from the chopped green beans and involves first
for about an hour. They are then placed in blanket adding water to the chopped beans. The temperature
lined cases where they are allowed to "sweat” for twenty of the water is normally about room temperature (25
four to forty-eight hours. The sweating process is re C.) but can be varied so long as the flavor producing in
peated a number of times after which the beans are gredients of the beans are not adversely affected. Addi
allowed to cool and age until cured. 50 tion of water is preferably in the approximate ratio of
The Bourbon process is essentially the same as the about three parts Water to two parts beans, by weight
Mexican process except for the fact that the beans are This
not exposed to direct rays of the sun and are initially and isratio can,only
defined of course, be varied
by practical over wide
expediency. limits
Sufficient
plunged into water near the boiling point. Both the water
Mexican and Bourbon processes take three to four months 55 Theshould water
be added to provide a workable mass.
and bean mixture is thoroughly agitated
to complete, and both are followed by extraction of by any suitable means. The mixture is then pressed
the cured vanilla, and, if desired, by concentration thereof. through a filter medium on which the bulk of the bean
The curing processes described heretofore, have been fibrous material is retained and the filtrate is reserved
improved upon in the past. For example, a process representing the first green bean extract.
involving pulping the green beans and then heating the 60 After this initial extraction, additional extraction steps
pulp in intimate association with air to effect a cure has are carried out, the exact number of which is deter
been perfected. Here again, however, extraction, and, mined only by the desire to insure substantially complete
when desired, concentration of the vanilla, follows cur
IIlg. extraction. Each of such additional steps involves wash
As noted heretofore, it has become apparent that an 65 by ing the fibrous material retained in the filter medium
undesirable loss in favor and odor occurs during con initial thoroughly mixing the same with water as in the
extraction.
ventional curing processes, and particularly during con variable and dependsAgain, the amount of water added is
upon practical considerations. The
centration of extracts of conventionally cured beans.
Therefore, the present invention contemplates a method mixture as was
is then filtered through the same filter medium
used for the first extract. The residue retained
by which curing is carried out after extraction and con O from these additional extraction steps is then discarded
centration of the vanilla extract since flavor and cdor. and the various filtrates are combined with the initial
 *2,835,591
3 4
filtrate and are either reserved for the following concen bean extract, the degree of concentration is governed by
tration step, or for immediate curing. commercial expediency, i. e., the less the degree of con
In connection with the last statement heretofore, con centration, the more evaporation that is required in the
centration is to be normally considered a part of our curing step.
process. Alternatively, immediate curing following ex Of course, in both instances noted heretofore, concen
traction is possible subject to the fact that, in the case tration should not be carried to such a great degree or
of our alternative liquid curing step described herein accomplished in such a manner as to commence curing
after, a dilute final extract is obtained. To amplify on of the green bean extract in the concentration stage.
this, vanilla extract made by our process is typically The next step in the process, step IV, involves curing
marketed as an extract of "multi' or "single' strength O the concentrated green bean extract. However, before
makeup. Such strengths require at least some concen curing, or, as a matter of. fact, during curing, one or
tration of green bean extract so that the concentration more enzyme systems, as, for example, pectinolytic, dia
step is necessary. However, omission of concentration static, proteolytic, glycosidases and catalase, in different
combinations and amounts, can be added to the green
from our process will result in a final extract which, 15 bean
although diluted below single strength, and not typically concentrate. These enzyme systems have been
marketable, is, nevertheless, a product of some utility and found to be of value in varying the taste, odor, physical
contemplated by our invention. and chemical characteristics of the final cured vanilla
In the case of utilization of our other curing step de extract.
scribed hereinafter, which involves evaporation of green 20 It has not been definitely ascertained as to the par
bean extract to dryness, we are not here faced with the ticular chemical phenomena that occur by the addition
attainment of a dilute final extract upon the omission of these enzymes. However, we have found, for example,
of the concentration step because, of course, the very that a proteolytic enzyme such as Rhozyme A-4, con
act of evaporating constitutes a type of concentration. tributes significantly to the desirable characteristics noted
Nevertheless, a separate preceding concentration step is 25 heretofore in the final cured vanilla extract. Other speci
still desirable because of the fact that evaporation of a ic enzymes that are contemplated, exemplified herein
non-concentrated large volume of extract would be com after.
mercially impractical. Pectinolytic: Pectinol. O
It should be noted that the extraction steps noted here Proteolytic: Rhozyme Al-4
tofore are also carried out in an oxygen-free atmosphere. 30 Cellulase, cellobiase, hemicellulase, gumase, pentosamase,
In addition, it can be stated that any suitable type of maltase: Enzyme 19
filter medium can be used. Lipase, esterase: Lipase B
As previously stated, the green vanilla beans and the Diastatic: Rhozyme R-48, Rhozyme S
green vanilla bean extract taken therefrom, have no Glucose-oxidase, catalase: DeeO
vanilla flavor or odor. The oxygen-free atmosphere 35 Amylase, dextrinase, maltase, protease, peptidase, renin,
helps to insure such conditions, since development of phosphotase, cellulase, sulfatase, invertase: Clarase 300
flavor and odor are desired to be postponed until the Catalase: Catalase
final curing step. B glycosidase: Emulsin
The make-up of the green bean extract comprises water,
and soluble and insoluble green vanilla bean solids. Of 40
Step IV of the illustrated flow chart, constitutes the
course, the exact composition is determined by the final curing step and achievement of cured vanilla extract.
amount of green beans initially utilized, the amount of Alternative steps have been found to work equally well
water used for extraction, and the degree of extraction and are designated IVa and IVb.
that is carried out. As pointed out heretofore, all of In step IVa the green bean concentrate is spread as a
these factors are variable dependent only upon practical liquid film on metal or glass trays. The trays are placed
and commercial expediency. 45 in a vacuum oven where they are subjected to heat. The
Subject to the above comments as to possible omission preferred temperature range is 60° C.-90° C. with about
of concentration step, the combined filtrates are then 75 C. being the optimum. The maximum temperature
conveyed to a vacuum concentrator wherein concentra range that can be considered operable ranges from 40
tion, which is step III of the process, occurs. The green C. to 110° C.
bean extract is placed in this concentrator and heated 50 The vacuum oven in which the concentrated green
under a vacuum to a temperature not substantially bean extract is placed is preferably under a vacuum of
greater than about 30° C. and preferably about 28° C. 35 to 100 mm. of mercury absolute, with 45 mm. being
The upper limit of 30° C. is subject to some variation . typical. The maximum working range can be considered
and it should be borne in mind that, in the final analy 55 to be from 35 to 350 mm. absolute.
sis, the temperature of concentration should not be so Curing in the vacuum oven under the above conditions
high as to adversely affect the flavor producing ingre is preferably carried out for a period of five-ten hours
dients of the green bean extract. As great a degree of with six hours being optimum. Again, the maximum
vacuum as commercially practicable is desired. time period range contemplated is one hour-twenty-four
The concentrator can be of standard design well known hours.
in the art. It contemplates the use of heat and high 60 During this curing step, the constituents which impart
vacuum. A vacuum of about 35 mm. of mercury abso characteristic flavor and aroma to vanilla are developed.
lute is preferred. It should be pointed out that the flavor and aroma char
The green bean extract is concentrated to whatever acteristics of vanilla, developed by both curing steps
volume is necessary in order that the final concentrated IVa and IVb, the latter to be described, correspond to
extract will be of required strength and in accordance 65 those developed in the presently used methods noted
with practical expediency. As noted heretofore in the heretofore, even though curing is not carried out until
case of liquid curing, the degree of concentration of after extraction and concentration. As a matter of fact,
extract determines, to some extent, the strength of the these beneficial characteristics are present to a far greater
final cured vanilla extract and, accordingly, is variable degree because of the fact that no loss of flavor, aroma,
depending on whether a dilute extract or one of at least 70 and the like occurs during the extraction and concentra
single final strength is desired. In any event, concen tion of the undeveloped green bean extract.
tration should be carried out to an extent sufficient to Following curing, the dry residue is scraped from the
permit the addition of at least some ethyl alcohol, pref trays and combined with ethyl alcohol and water to
erably 35% of final volume of cured vanilla extract. produce a final cured extract of desired strength. After
In the case of curing involving evaporation of green 75 the residue is thoroughly mixed with the alcohol, it is
 2,835,591
5 6 -
allowed to stand until all soluble material is dissolved. Concentration
At the end of this time, the liquid is filtered to remove
all insoluble particles and the resulting liquid is an ac The 3650 cc. of liquid was concentrated in a laboratory
ceptably cured extract. concentrator under a reduced pressure of 35 mm. of
In step Vb, the green bean concentrate of step III mercury, at a temperature of 29 C., to a volume of 1000
is cured by heating in a vessel at a preferred temperature cc. The concentrate was divided into five portions of
of 55-80 C. with 60° C. being typical. Although a 200 cc. each. Two of the 200 cc. portions of concentrate
preferred temperature range has been set forth, maximum were reserved for curing by the following methods.
range of 20 C-100° C. is contemplated. First portion (cured to dryness in vacuum oven)
The concentrate is heated for a preferred time period 0 Concentrate in the amount of 200 cc. was spread out
of 48-150 hours, with 50 hours being typical. Again, in a thin film, A6' thick, upon aluminum dishes, and
the preferred range is set forth, but a maximum range of placed in a vacuum oven under a reduced pressure of
12 hours-300 hours is contemplated. 50 mm. of mercury, at a temperature of 70° C. for a
Heating can be achieved in imany ways. For example,
the green bean extract may be placed in a tank with a 5 period of six hours. At the end of this time, the dried
coiled pipe mounted therein. Hot water, which may be Vanilla solids were scraped from the aluminum dishes
and combined with ethyl alcohol and water to 400 cc.
thermostatically controlled to maintain the desired tem total, with the final concentration of alcohol being 40%
perature within the tank, is circulated through the coiled by volume. This solution was then filtered through a
plpe.
Throughout the heating period, an inert gas such as 20 The Bichner funnel to remove insoluble suspended particles.
nitrogen, mixed with oxygen, is bubbled through the loss in volume due to removal of such particles was
insignificant.
concentrate. The preferred amount of oxygen is Enough alcohol and water were added to yield a final
1%-20% of the total volume of gas with 5% being extract of 'single” strength. Since we know the total
typical. However, 0.1%–30% oxygen is contemplated volume of finished single strength extract that the be
as the broadest range. ?' 25
ginning weight of beans would produce based on accepted
The gaseous mixture can be applied to the concentrate definition and on the extraction steps carried out, it
in many ways, e.g., by delivery through a plurality of Was then possible to determine the amount of alcohol and
holes in the bottom of the tank aforesaid. The gas is Water to be added to achieve such volume.
pumped into the tank and thus intimately mixed with the
concentrate as it is being heated. r Second portion (cured as a liquid)
At the end of the curing period, the cured concentrate Concentrate in the amount of 200 cc. was held in a
is mixed with ethyl alcohol. Water can also be added glass vessel at a temperature of 55° C. for 48 hours.
with the alcohol and the solution is allowed to stand until during that time a mixture of nitrogen and oxygen (5%
all soluble material is dissolved. The solution is then oxygen) were bubbled through the material. At the end
filtered to reiflove insoluble particles and the resulting 35
of the curing, the 200 cc. of cured concentrate was com
extract is in final acceptable form. bined with alcohol and water to a final volume of 400
Of course, the final volume of extract is primarily cc. (40% ethyl alcohol). The cured extract was then
dependent upon the amount of starting material, the filtered to remove insoluble particles, with the resulting
degree of extraction, and final fold strength desired. extract considered to be single strength.
These features determine the amount of alcohol and 40 The final volume of 400 cc. in both instances was
water added in curing steps Va and IVb with the alco determined by considering the following:
hol representing about 35% of volume in the final cured It should be noted that the original 1200 grams of
extract. This latter figure can vary, but has been found green vanilla beans is approximately equivalent to 200
to be commercially desirable. - grams of cured dried vanilla beans, and 200 grams of
EXAMPLES cured dried vanilla beans can make 2000 cc. of single
strength vanilla extract after substantially complete ex
initial extraction (oxygen-free atmosphere) traction is carried out. When a 200 cc. portion of the
1200 grans of fresh, whole, mature finely chopped i000 cc. of concentrate was removed for curing, this
green vanilla bears (80-90% moisture) were agitated in 50 portion contained one-fifth of the extractable matter of
a large Waring Bleidor (4 quart capacity) with 800 cc. 1200 grams of green vanilla beans or 200 grams of cured
of water, at room temperature (25 C.), for about three dried beans. This is equivalent to 240 grams of green
minutes. The resulting mixture was filtered through four beans or 40 grams of cured dried beans. 40 grams of
layers of cheese cloth, with the liquid passing through beans cured and dried is equivalent to 400 cc. of single
the cloth being reserved to be combined with water washes, 55 strength extract (based on U. S. Department of Agricul
and the residue on the cloth, after being pressed to re ture definition hereinafter set forth).
move liquid entrapped therein, was reserved for the The two examples cited both end up with a single
first wash. strength extract. This was done in these experiments
First wash for convenience in order to more easily evaluate the
60 quality (taste and odor and chemical properties) and
Residue from the initial extraction was agitated in compare them with existing single strength extracts which
the Waring biendor with 600 cc. of water at room tem can be considered to be standards.
perature (25 C.) for about three minutes. The result The present process of preparing vanilla extract is a
ing material in the blendor was filtered through four radical departure from former processes, because extrac
layers of cheese cloth, with the filtrate being reserved to 65 tion and concentration of green bean extract are initially
be combined with the initial extract and later washes, carried out followed by curing of the concentrated green
and the pressed filter cake being reserved to be used in bean extract in that form. Processing of the green bean
the succeeding wash. extract, as described, prevents the destruction and dissipa
Second and third washes tion of the natural volatile oils and other constituents
which contribute the aroma and flavor characteristics of
These washes are identical with wash if 1 in volume, 70 vanilla. The process, therefore, results in a final vanilla
temperature of water, and time of agitation. extract of richer flavor and aroma than previously ob
After the extraction and subsequent washes were com tained.
pleted, all of the filtrates were combined to give a final It should additionally be noted that our process is
volume of 3650 cc. This liquid was reserved to be used
in the concentration. 75 much more economical than previous methods, since the
unusable portions of the bean are eliminated early in the
 2,835,591
7 8
processing. This lowers the cost of such factors as water, said alcohol and water being added in amount
handling, time expended, and the like. sufficient to produce a cured vanilla extract of desired
The definition of “single' strength for the purposes strength.
of this specification is the extractab?e matter from 10 13. The method of claim 12 wherein evaporation is car
grams of cured and dried vanilla beans per 100 cc. of ried out at a temperature of from about 60° C. to about
cured vanilla extract. 90° C. and for a time period of from about five hours
As noted heretofore, although preferred ranges of tem to about ten hours.
perature, time, vacuum conditions, concentration and the 14. The method of claim 12 wherein the residue-alco
like have been set forth, broader ranges are many times hol-water material is allowed to stand for a time suffi
contemplated. It must be understood that the invention O cient to dissolve substantially all soluble material, and
is not limited to preferred ranges so long as the desired , thereafter the said mixture is filtered to remove all
results are effected. The invention includes all variations insoluble particles.
in procedures covered by the appended claims and their 15. The method of claim 11 wherein the said curing
equivalents. and alcohol addition stages comprise heating the said con
We claim: centrated green bean extract while coincidentally bubbling
1. The method of producing cured vanilla extract from an inert gas and oxygen therethrough, and thereafter
green vanilla beans which comprises extracting green bean adding water and alcohol to said extract.
extract from green vanilla beans substantially in the 16. The method of claim 15 wherein heating and gas
absence of oxygen, then curing the green bean extract to treatment are carried out at a temperature of from about
thereby produce a cured vanilla extract of greatly en 20 55 C. to 80° C. and for a time period of from about
hanced flavor and aroma. forty-eight hours to one hundred fifty hours.
2. The method of claim 1 wherein ethyl alcohol and 17. The method of claim 15 wherein the inert gas is
water are added to the extract following curing and in nitrogen and wherein the oxygen is in amount of from
amount sufficient to produce a cured vanilla extract of about 1% to 20% of the total volume of nitrogen and
desired strength. 25 Oxygen.
3. The method of claim 2 wherein the said curing 18. The method of claim 15 wherein said water
and alcohol-water addition stages comprise evaporating alcohol-extract mixture is allowed to stand for a time
the green bean extract to dryness in a vacuum to form a sufficient to dissolve substantially all soluble material and
cured residue and combining the residue with alcohol and thereafter filtered to remove all insoluble particles.
Water. 30 19. The method of claim 11 wherein said chopping
4. The method of claim 3 wherein evaporation is and extraction stages comprise chopping up mature green
carried out at a temperature of from about 40 C. to vanilla beans, adding cold water to the chopped beans to
110° C. and for a time period of from about one hour to thereby form a first bean-water mixture, thoroughly agi
twenty-four hours. tating and mixing the said first bean-water mixture, pass
5. The method of claim 1 wherein said curing step 35 ing the said first bean-water mixture through a filtering
comprises heating said green bean extract while co medium to thereby provide a first filtrate and filtered solid
incidentally bubbling an inert gas and oxygen there material, washing the filtered solid matter by adding addi
through. tional cold water thereto and agitating the same to there
6. The method of claim 5 wherein heating and gas by form a second water-bean mixture, passing the second
treatment are carried out at a temperature of from about 40 water-bean mixture through the same filtering medium
20° C. to 100° C. and for a time period of from about as was used on the first water-bean mixture to thereby
twelve hours to three hundred hours. provide a second filtrate, repeating the last two recited
7. The method of claim 5 wherein the inert gas is Washing and filtering steps and thereafter combining the
nitrogen and wherein the oxygen is in amount of from resulting filtrates to form the extract.
about 0.1% to 30% of the total volume of nitrogen and 45 20. The method of claim 19 wherein water in the water
oxygen. addition steps is added in amount of about 3 parts water
8. The method of claim 1 wherein at least one enzyme to 2 parts beans by weight.
system is added to the green bean extract following ex 21. The method of claim 11 wherein said concentra
traction. tion stage comprises heating said extract under a vacuum
9. The method of claim 1 wherein substantially all 50 at a temperature of not more than 30° C.
the green bean extract is extracted in the extraction stage. 22. The method of claim 11 wherein at least one enzyme
10. The method of claim 1 wherein a cured vanilla System is added to the green bean extract following con
extract of single strength is produced. centration thereof.
11. The method of producing cured vanilla extract from 23. The method of claim 11 wherein substantially all
green vanilla beans which comprises extracting green the green bean extract is extracted in the extraction
bean extract from green vanilla beans substantially in the Stage.
absence of oxygen, concentrating said extract under a 24. The method of claim 11 wherein a cured vanilla
vacuum, then curing the concentrated extract and adding extract of single strength is produced.
ethyl alcohol to thereby produce a cured vanilla extract 60 References Cited in the file of this patent
of greatly enhanced flavor and aroma.
12. The method of claim 11 wherein the said curing UNITED STATES PATENTS
and alcohol addition stages comprise evaporating the con 1,515,714 WuSSOW ––––––––------ ???. 18, 1924
centrated extract to dryness in a vacuum to form a cured 2,601,635 Romagnan ------------ June 24, 1952
residue and combining the cured residue with alcohol and 65 2,621,127 *------------------ Dec. 9, 1952