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OFF FLAVOR DEVELOPMENT IN CANNED APPLE SAUCE

By

WILLIAM VAN HODGE

AN ABSTRACT

Submitted to the College of Agriculture, Michigan State University of
Agriculture and Applied Science in partial fulfillment of
the requirements for the degree of

MASTER OF SCIENCE
Department of Food Technology

1959

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WILLIAM VAN HODGE ABSTRACT

A study was carried out during the winter and spring of 1959, to in-
vestigate the effect of temperature and length of storage on eighteen single
variety apple sauces. The apples had been harvested at the proper stage of
ripeness and stored at 32 to 34°F. Thirty pounds of fresh, sound apples
were selected from each of the varieties used and made into apple sauce
under simulated commercial conditions. The sauce was then adjusted to 17
percent soluble solids with sucrose and a representative sample of each
sauce was frozen, to serve as control. The remainder of the sauce was
canned in No. 303 cans and divided into three lots. These lots were stored
at 32° F, 70 to 75’F, and 85’F. The 85‘ F lot was stored at this higher tem-
perature to accelerate the development of storage effects.

The results of the measurements made on the apple sauce stored at
various temperatures indicate that the development of the off flavor com-
ponent, n-caproic acid, is a function of time and temperature. This de-
velopment continues to increase quite rapidly for some time, then gradually
tends to level off. The tin content and caproic acid content play a role in
the development of off flavor and dark color in apple sauce.

These are not the only factors responsible for off flavor since sauces

stored at 85° F had comparable amounts of tin and caproic acid as that stored

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WILLIAM VAN HODGE ABSTRACT-2

at 70°F and both exhibited off flavor, but the sauce stored at 85°F was much
more undesirable in this respect, and also showed darkening of the sauce.
No explanation for this can be given at this time. There was considerable
variation in the amount of caproic acid developed among the various varie-
ties tested.

There was small differences in pH, total acidity, acetaldehyde,
amide N, soluble solids, consistency, viscosity and tin content with little
or no change in the quantities of the factors during storage, except in the
case of tin, which tended to increase with increased storage time. No
relationship could be found between these factors and the development of

caproic acid.

OFF FLAVOR DEVELOPMENT IN CANNED APPLE SAUCE

By

WILLIAM VAN HODGE

A THESIS

Submitted to the College of Agriculture, Michigan State University of
Agriculture and Applied Science in partial fulfillment of
the requirements for the degree of

MASTER OF SCIENCE

Department of Food Technology

1959

ACKNOWLEDGEMENTS

The author is deeply indebted to Dr. Clifford L. Bedford for his
assistance in conducting this study, his aid and advice in analyzing the data,
and for his counsel in the preparation of the manuscript. The author also
wishes to express his sincere appreciation for the assistance given him by
Drs. George Borgstrom, Otto Bunneman, Karol Kropp, and Messrs. W. F.
Robertson and H. A. Cardinell without which this study would not have
been possible. Appreciation is expressed to the graduate students who

assisted in the analyses of the samples.

 

 

RE

TABLE OF CONTENTS

INTRODUCTION . . .......... . . ........
REVIEW OF LITERATURE . . ........... . .
METHODS AND MATERIALS . . ............
MEASUREMENTS AND DESCRIPTIONS ............
pH and Total Acidity ..................
pH and Volatile Acid Content . . . . . . . .....
Identification of the Volatile Acid Component. . .....
Acetaldehyde. . . . . . ........... . . . .
Ammonia N and Amide N ...............
Soluble Solids . . . ..................
Consistency and Viscosity ....... . . ......
Tin Content ........ . ...........
RESULTS AND DISCUSSION . . . . . . . ..........
Off Flavor Component ....... . . ........
Consistency. ...... ...............
pH and Total Acidity ........ . . . . ......

SolubleSolids.....................

Tin.... ................... ...

10

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12

12

12

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17

17

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TABLE OF CONTENTS CONT'D

Page

Acetaldehyde ...................... 22
Ammonia N and Amide N ................ 24
SUMMARY AND CONCLUSIONS ................ 26

BIBLIOGRAPHY. . . . . . . . ................ 28

INTRODUCTION

The canned apple sauce industry has expanded considerably in recent
years, and apple sauce has become one of the important processed foods in
the United States. In 1940 the United States pack was 2, 364, 864 cases (#303
equivalent), and in 1958-59, 16, 002, 901 cases, which was an increase of
nearly a million cases per year. The 1958-59 pack of apple sauce was equal
to about 49 percent of the canned peach pack of that year (5). The main areas
of production are California, Washington and Oregon in the western part of
the United States, and New York, Pennsylvania, Maryland, Virginia and
West Virginia in eastern United States. Although apple sauce is produced
in large quantities in Michigan, it has not as yet become a major processed
item in this State.

Cruess (9) has reported that owing to the change in consumer demand
nearly all of the Gravenstein variety in California is now being used in the
production of apple sauce. This is being generally reflected in all areas,
as there has been a steady decline in the per capita consumption of all varie-
ties of fresh apples (a decrease from 27. 6 pounds per person in 1936 to 19. 2
pounds in 1957), and an increased consumption of processed apples (an increase
from 2. 8 pounds per capita to 6. 9 pounds) (7).

The varieties of apples used in the production of apple sauce vary

with the area of production. In California, the Gravenstein variety is the one
used chiefly for sauce (9), while in New York, Pennsylvania, Maryland and
Virginia blends of such varieties‘as York, Jonathan, Golden Delicious, Rome
Beauty and Stayman are used in their apple sauce.

Recently it has been reported (17) that canned apple sauce develops
an "off flavor" described as "tinny" or " goaty” during storage. Because of
the fact that flavor is one of the important quality factors in selling apple
sauce, a study was made to determine the effect of temperature and length
of storage on the development of off-flavor in apple sauces produced from
eighteen varieties of apples grown commercially in Michigan. This study

was undertaken during the winter and spring of 1959.

REVIEW OF LITERATURE

Commercially packed apple sauce is a relatively new processed food,
being about forty years old. It is believed that the Barlow Brothers Canning
Company was the first commercial processor of apple sauce, using modern
methods of processing.

Apple sauce is prepared from sound fresh apples (Pyrus malus) of

 

the proper ripeness. The apples are washed, peeled and cored, trimmed,
sorted, chopped or sliced, blanched, and pulped (2, 6, 9, 10, 21). The sauce
may or may not contain added sweetening, water, salt and spices, and is
sufficiently heat processed to assure preservation (25). Heating of the
chopped or sliced apples is generally accomplished by one of two methods- -
direct steam injection or with the conventional steam jacketed kettle process.
The former method is in much wider commercial usage, and the Allen type
processing equipment is most commonly used. It is preferred because it
provides a rapid, efficient and easily controlled procedure.

It has been reported by several researchers (2, 6, 21, 26) that the
quality of apple sauce is determined by four factors- -flavor, color, consis-
tency, and absence of defects. Flavor has been considered the most impor-
tant of these factors, although color and consistency play a very important

role. Pfund (21) reported that in addition to sweetness and a moderate degree

of acidity, odor was also important in determining the flavor of apple sauce.

Power (22) working with fresh apple parings, isolated amyl alcohol,
formic, acetic, caproic and caprylic acids, and concluded that the odorous
constituents of apples consisted of amyl esters of the above named acids.
More recent work (15, 16, 28) has shown the presence of primary alcohols
from one to six carbon atoms, aldehydes, ketones and esters of formic,
acetic, propionic, butyric and caproic acids in stored apples, which contri-
bute to the volatile fraction of the apple flavor. It is recognized that during
the manufacture of apple sauce some of these volatile compounds are lost
in the cooking and filling processes. The result is a lack of typical apple
flavor in the sauce (17). It has been suggested (4) that apple essence be
added to the sauce in order to replenish the lost flavor.

In addition to flavor lost during processing, it has been reported that
apple sauce during storage develops a flavor and aroma which is disliked
by the consumer (I), and described as "rank or tinny". Mattick, Moyer and
Shallenberg (17) have isolated n-caproic acid from stored canned apple sauce.
They tested sauces. made from Baldwin and McIntosh apples, and from blends
of Rhode Island Greening, Baldwin, Ben Davis, Northern Spy and Wealthy,
and of Baldwin, Cortland, Rome Beauty, and found n-caproic acid in concen-
trations up to 120 ppm, depending on storage time. They concluded that it

was largely responsible for the rank flavor of apple sauce. The source of

caproic acid is not known. The amount of caproic acid isolated from esters
in apple essence by White (29) appears to be too low to account for the
amount found in apple sauce.

Flavor changes in canned apple sauce have also been reported as due
to changes in the non-volatile constituents (acids, sugars and salts) (21, 26).
Pfund (21) and others reported that during storage the total acid content tends
to decrease and result in flatness. This was particularly noticeable in some
varieties, such as the Golden Delicious.

Sugar content also plays an important part in the flavor of the apple
sauce (6, 21, 26, 28). Dryden and Hills (10) found that a sugar content of about
22 percent with an acid content of 0. 45 percent was preferred. If the acid
content was increased or decreased, a corresponding change in sugar content
was necessary.

Although consistency is recognized as an important factor in apple
sauce quality, no objective method of measurement is recognized in the
present standard (2). Consistency measurements have been reported, by
using the line spread procedure (6, 9, 21, 26, 27, 28) with the Stormer viscosi-
meter (13, 15, 28) and with the Brookfield viscosimeter (15). It is indicated
that a measurement of consistency would be useful to detect undesirable

changes (28).

METHODS AND MATERIALS

The eighteen apple varieties used in this study are as follows:
Baldwin, Ben Davis, Caville Black, Cortland, Fameuse, Golden Delicious,
Grimes Golden, Jonathan, McIntosh, Northern Spy, R. I. Greening, Stark,
Stayman, Tolman Sweet, Wagener, Wealthy, Winter Banana and Wolf River.
They were obtained from Michigan State University orchard during the
fall of 1958, and were stored at 32’ Ft 1°F with a relative humidity of 851' 5 per-
cent. All varieties were stored about four months before processing. The
apples were removed from storage and held at room temperature for three
hours prior to sorting and processing. Thirty pounds of sound apples of
each variety were used in the preparation of sauce. The apples were
washed, peeled, cored and cut into twelths. The prepared slices were
covered by cold tap water (57°F) until processed, to minimize browning.

The sliced fruit was steam blanched for three minutes to soften the flesh

and to stop enzymatic activity. They were immediately pulped in a laboratory
size Langsenkamp pulper, using a 3/32 inch screen. The sauce was adjusted
to a soluble solids content of 17 percent, and the sweetened sauce was filled
hot into #303 (apple sauce) cans, given a 7-minute exhaust, closed and hot—
water processed five minutes. Representative samples of sauce of each
variety was taken prior to processing and put into plastic containers and

frozen, to serve as checks.

After cooling the cans in running cold water, each lot of apple
sauce was divided into three lots; one lot was stored at 32°F, one lot at
70 to 75°F, and the third lot at 85° F. The higher temperatures were

used to accelerate the effect of storage conditions.

MEASUREMENTS AND DESCRIPTIONS

pH and Total Acidity

A ten- gram representative sample of apple sauce was thoroughly
mixed with 200 m1 of freshly boiled, cooled, distilled water, and the pH

determined, using a Beckman Zeromatic glass electrode pH meter. The

sample was then titrated to a pH of 8. 2 and the results expressed as per-
cent malic acid. In the pH determination it was found necessary to add at

least a small quantity of freshly boiled distilled water to assure even distri-

bution of the hydrogen ions. The optimum quantity of distilled water was

found to be 200 ml for both pH and total acidity determinations. Initial

studies showed the pH values obtained on the dilute sauce were the same

as those obtained on the undiluted sauce.

pH and Volatile Acid Content

The procedure for the distillation of volatiles was similar to that
described by Mattick 9.23.1; (17). A 100- gram representative sample of
sauce was weighed into a 500 ml round bottom boiling flask with 50 m1 of
freshly boiled distilled water and steam distilled at the rate of 5 ml per
minute until 200 ml were collected. The steam generator consisted of a
3 liter flask with a 3 necked top, fitted with an internal coil of nichrome

wire immersed in boiled distilled water and regulated with a variable voltage

transformer. The distillate was condensed with a Allihn condenser, and

collected in a beaker containing 50 ml of freshly distilled water. The dis-

charge tip of the condenser was placed below the surface of the water in

the collection beaker, and the beaker was placed in an ice water bath to

minimize the loss due to volatilization. The pH of the distillate was de-

termined, using a Beckman Zeromatic glass electrode pH meter, and then

titrated to a pH of 8. 2 with (0. 01 N NaOH) to determine the volatile acid

content of the sauce. The results were expressed as mg of n-caproic acid

per 100 grams of sauce.

Identification of the Volatile Acid Component

The procedure used for the quantitative identification of the volatile
component was similar to that described by Block e_t 11: (3). The titrated
samples were concentrated about 1, 000 times to obtain a sample of the
sodium salt of the acid sufficiently large for the chromatographic identifi-
cation procedure. The sodium salt of the acid was converted to an ammonium

salt to eliminate the possibility of the acetic spots being masked or obliter-

ated by the sodium ion. The ammonium salt of the acid was spotted on

Whatman's No. 4 chromatographic paper, and developed with the solvent
(1 part concentrated NH4OH and 100 parts 95% CZHSOH). The chromato-
gram was dried and sprayed with bromophenol blue indicator (50 mg of

indicator in 100 ml of water plus 200 mg of citric acid). The presence of

10.

ammonium salts was indicated by the appearance of blue spots on a yellow

background.

Acetaldehyde

The procedure and apparatus for the separation of acetaldehyde from
apple sauce was similar to the steam distillation procedure described by
Mattick e_t _a_l: (17). The quantitative determination of acetaldehyde was sim-
ilar to that described by Joslyn e_t a_l_. (14). A 200 ml sample of the steam
distillate was placed into a 500 ml Erlenmeyer flask containing 50 ml of a
neutral buffer solution (3. 35 grams KH2P04 plus 15 grams Na2P04- 12 H20
per liter) and 10 ml of bisulfite solution (18. 9 grams anhydrous Na2803 and
150 ml of N. H2804 per liter). The flask was stoppered and shaken. After
standing for 20 minutes, 1 ml of freshly prepared 1% starch solution and
10 m1 of acid solution (250 ml concentrated HCl per liter) were added. The
excess bisulfite was then titrated with 0. IN iodine solution until a blue end
point was reached.

The solution was then made alkaline by adding 100 ml of an alkaline
buffer (8. 75 grams H3w3 and 400 ml of 1N, NaOH per liter). This liberated
the bound bisulfite and the blue color. disappeared. The solution was then

titrated with 0. DIN iodine solution until the blue end point returned. A blank

was run on the reagents using 100 m1 of distilled water. (1 ml of 0. 01 N

iodine = . 22 mg acetaldehyde).

ll.

Ammonia N and Amide N

The procedure used for the determination of ammonia and amide
nitrogen content of apple sauce was similar to that described by Pucker _e_t _a_l_.
(23) except the quantitative determination was made titrametrically. A

representative 100 gram sample of apple sauce was blended with 100 ml of

distilled water for two minutes, then filtered through E and D No. 619 folded
20 cm filter paper.

For ammonia N, a 50 ml representative sample of the water extract
was transferred to a 500 ml Kjeldahl flask in a 55°C water bath and 5 ml of
a saturated sodium borate solution (pH 10) was added. The sample was
aerated for 15 minutes at the rate 2-3 bubbles per second with an air inlet

tube and the distillate was condensed and collected in a beaker containing

5 ml 0. 1 N. HCl and 20 ml of distilled water. The residual acid was titrated

with 0. I N NaOH using methyl red as an indicator.

For amide N, a 20 m1 representative sample of the water extract was
transferred to a 500 ml Kj eldahl flask and 2 ml 6N. H2804 added. The mix-
ture was refluxed on a steam bath for three hours, cooled and then the acid
was partially neutralized by the addition of 10 ml of 0. l N. NaOH. The re-

mainder of the procedure used for amide N determination was the same as

that used for ammonia N determination.

12.

Soluble Solids

The soluble solids content was determined with an Abbe refracto-

meter on the liquid obtained by expressing a representative sample of apple

sauce in a double layer of cheese cloth.

Consistency and Viscosity
Consistency and viscosity measurements were made at 70°F with a

Bostwick consistometer and Brookfield Synchro Lectric viscosimeter. The

Bostwick consistometer measurement results were expressed as cm of

flow in 15 seconds. The Brookfield viscosimeter was operated at 12 rpms

using a No. 4 spindle with the sauce filled to a depth of 3 1/2 inches in tall

200 ml beakers, the results expressed as relative viscosity measurements

(centipoise).

Tin Content

The procedure used for the quantitative determination of tin in canned

apple sauce was similar to that described by Morris _e_t El. (20).
A representative 25 gm sample was weighed into a 800 ml Kjeldahl
flask and 10 to 15 ml concentrated H2804 and 50 ml concentrated HNO3 were

added. The flask was then heated until all brown fumes had dissipated and

the volume of the water white solution was 10 to 15 ml. It was necessary

to add additional 5 to 10 m1 of concentrated HNO3 in order to obtain a water

13.

white solution. The Kjeldahl flask was cooled and a small quantity of
KCIO3, 15 ml concentrated HCl, and 10 m1 H20 were added, after which
the flask was heated until white fumes appeared and the solution was clear.
The contents were then transferred to a 300 ml Erlenmeyer flask and 25 ml
of concentrated HCl and 0. 5 grams of aluminum foil was added. The flask
was connected with a rubber stopper and glass tube to a beaker containing

10% KHCO3, and the hydrogen gas allowed to escape through the KHCO3

solution. The flask was then cooled in an ice water bath which drew in a

small quantity of the KHCO3. The partially neutralized contents of the flask

were immediately titrated with 0. DIN 12 and the results expressed as mg

Sn. per 100 grams of sauce.

14.

RESULTS AND DISCUSSION

Off Flavor Component
The main, rank, volatile component found in the steam distillate

was identified as n-caproic acid by the use of paper chromatography pro-

cedure. This is in agreement with the results reported by Mattick et al_. (17).

No other volatile acids were found.

Since the volatile acidity of apple sauce was found to be caproic acid,

steam distillation of this component and titration offered an efficient routine

procedure for its measurement. However, to obtain comparable results

between replicate samples, it was necessary to carefully standardize the

method as to the rate of distillation (5 ml per minute). Distilling at this

rate and collecting 200 ml of distillate, the recovery of added n-caproic acid

was from 98 to 101 percent. Faster rates of distillation resulted in varia-

tions in the amount of caproic acid recovered and lower rates gave incomplete

recovery even when the amount of distillate collected was increased to 500

ml. No explanation can be given for the erratic recovery at the faster rates
of distillation, but condensation of the steam in the boiling flask was the major

problem at the lower distilling rates.
As shown in Table I, the amount of n-caproic acid formed during

storage differed considerably between apple varieties. The largest amount

15.

was formed in the sauce made from Wealthy apples. Mattick eta}; (17)

reported that the concentration of caproic acid ranged from 0 to 12 mg per

100 grams of apple sauce. No explanation can be given as to the differ-

ences found between the varieties, since the source of the caproic acid is

not known. The rate of development of caproic acid varied with the time

and temperature storage (Table D. The average caproic acid content of

the apple sauces stored at 32°F for 84 days was similar to those stored at

70°F for 42 days, or at 85°F for 35 days. The results indicate that the

amount of caproic acid formed tended to increase linearly with time up to
70 and 56 days at 70 to 85°F respectively. Further storage of 21 days at
85°F showed only slight increase in the caproic acid content indicating a
leveling off in its formation. Mattick _et a_l. (17) found a linear relationship
between storage time and caproic acid formation for sauces stored at 20° C

for 22 weeks.

The odor and taste of apple sauce stored at 70°F was not considered

unpleasant after 70 days of storage, but the taste of sauce stored at 85°F

became objectionable after 56 days, and both odor and taste were very ob-

jectionable after 77 days. An odor similar to that found in apple sauce

stored for 77 days at 85°F was obtained when 11 mg SNC12 and 11 mg n-
caproic acid were mixed with a 25 gm sample of thawed frozen apple sauce.

This indicates that tin and caproic acid play a role in the development of the ob-

jectionable odor and flavor of canned apple sauce.

TABLE I

Caproic Acid Formation in Canned Apple Sauce

 

Storage Temperature

 

 

 

 

 

Variety -5°F 32°F 70°F 85°F X332:
49 days 84 days 42 days 63 days 70 days 35 days 56 days 77 days
m g/ 100 gram 31/
Baldwin 2.9 6.6 7.5 11.7 12.0 8.8 15.6 15.7 11.1
Ben Davis 3. 0 9. 0 5. 8 12. 5 13. 0 8. 7 18. 0 18. 0 12.1
Caville Black 2. 7 6. 5 6. 4 7. 8 8. 5 8. 6 13. 8 14. 4 9. 4
Cortland 3. 5 7. 8 6. 7 12. 8 12. 5 7. 6 17. 1 17. 5 11. 7
Fameuse 3.8 11.2 6.8 9.0 9.7 8.4 II. 9 12.5 9. 9
Gold. Delicious 3. 2 10. 7 6. 7 9. 3 9. 7 6. 3 14. 7 14. 5 10. 3
Grimes'Golden .3. 9 8. 9 5. 4 11. 4 11. 6 6. 3 15.2 15. 7 10. 7
Jonathan 3. 9 8. 2 5. 9 10. 4 10. 7 6. 3 6. 8 17. 1 9. 3
McIntosh 3. 5 7. 6 6. 5 10. 5 12. 4 8. 8 15. 5 15. 6 10. 9
Northern Spy 3.5 7.6 9.4 11.4 12.1 9.1 14.0 15.3 11.3
R. LGreening 3.1 6.0 8. 7 13.1 13.7 11. 3 13.4 17. o 11.9
Stark 2.0 6.1 6.8 11.7 12.4 8.2 17.0 17.0 11.3
Stayman 3.1 6. 4 7. 3 11. 6 12. 2 6. 3 14. 7 15.1 10. 5
Tolman Sweet 2. 7 7. 9 2. 9 6. 2 7. 6 2. 9 9. 6 10. 2 6. 8
Wagener 2. 6 7. 4 4. 2 8. 4 9. 0 6. 7 10. 7 12. 2 8. 4
Wealthy 3.0 10.0 8.4 11.6 12. 1 11.5 16.6 16.0 12.3
Winter Banana 2. 5 7. 2 516 5. 8 6. 9 6. 7 11. 3 13.6 8. 1
Wolf River 2. 7 6. 4 8. 5 12. l 12. 5 9. 3 16. 5 16. 8 ll. 7
Average 3. 0 7. 8 6. 6 9. 7 11. 0 7. 9 14. 6 15. 3
l/

- Each datum represents the average value of 3 determinations.

given in the appendix table.

Individual values

l7.

Consistency

There was considerable difference between the consistencies of the
sauces made from the various varieties (Table II). This indicates that to
obtain uniform consistencies for the sauces made from various varieties of
apples, it would be necessary to adjust the amount of water added during

the processing operation.

pH and Total Acidity

 

There was no appreciable changes in pH or total acidity during
storage of individual varieties and their controls (Tables III and IV). The
greatest variation was between the total acidities of the varieties and

ranged from 0. 1 to 0. 55 percent malic acid. No significant relationship

was found between acidity and caproic acid production. (I = . 420).

Soluble Solids

 

There was no change in soluble solids content during the storage
of the sauce. The variations in soluble solids contents of various varieties
were due to experimental error in the soluble solids content adjustment

prior to processing (Table V).

Tin

 

There was considerable variation in the tin content from various

varieties. Fameuse, Caville Black, Wagener, Wealthy and Winter Banana

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93c 93.6 9:8 9:8 Pawn and misc gap 936 mind awn Tame mime 9:3 9:8 mime
N.Nl on mm 2. no N... em 3. FN. om mm on me Nv 3w 3.
9.3 meow “_on mam- momw moon mon mom-
6.453386% 3:396 3333.28. “3meon fimfiflw
zocoumwmcoU NAN—_moomtr
602mm 633. Ho zoaoumwmcoo lIIIII

: mags

TABLE III

pH of Canned Apple Sauce

Storage Temperature

 

 

 

 

 

Variety - 5° F 32° F 70° F 85° F

49 84 42 63 70 35 56 77
days days days days days days days days

Baldwin 3. 71/ 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7

Ben Davis 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7

Caville Black 3. 8 3. 8 3. 8 3. 8 3. 8 3. 8 3. 7 3. 7
Cortland 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7
Fameuse 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5
Golden Delicious 4. I 4. 0 4. 0 4. 0 4. 0 4. 0 4. 0 4. 0
Grimes Golden 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7
jonathan 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7
McIntosh 3. 8 3. 7 3. 7 3. 7 3. 7 3. 7 3. 8 3. 8
Northern Spy 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5
R. I. Greening 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5 3. 5
Stark 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 6 3. 7
Stayman 3. 6 3. 5 3. 5 3. 5 3. 6 3. 5 3. 5 3. 6
'olman Sweet 4. 6 4. 6 4. 6 4. 6 4. 6 4. 6 4. 6 4. 6
agener 3. 8 3. 8 3. 8 3. 8 3. 8 3. 8 3. 8 3. 8
2althy 3. 7 3. 6 3. 6 3. 6 3. 7 3. 6 3. 6 3. 6
nter Banana 3. 8 3. 7 3. 7 3. 7 3. 7 3. 7 3. 7 3. 6
>lf River 3. 5 3.4 3.4 3.4 3.4 3.4 3.4 3. 4

l_‘
I

l/
— Each datum

represents the average of two determinations.

l9.

TABLE IV

Total Acid of Canned Apple Sauce

 

Storage Temperature

 

 

 

 

 

 

Variety -5° F 32° F 70°F 85' F 1:13;:
49 84 42 63 70 35 56 77
days days days days days days days days
gm malic aCid/IOO grams

Baldwin . 341/ . 35 . 35 . 35 . 37 . 34 . 37 . 37 . 35
Ben Davis .35 .36 .39 .37 .38 . 36 .36 .37 . 36
Caville Black . 38 . 37 . 37 . 36 . 38 . 37 . 42 . 41 . 38
Cortland . 31 . 33 . 36. . 34 . 35 . 34 . 34 . 34 . 34
Fameuse . 33 . 36 . 34 . 38 . 35 . 34 . 38 . 35 . 34
Golden Delicious . 25 . 26 . 27 . 27 . 28 . 27 . 27 . 26 . 26
Crimes Golden . 26 . 27 . 27 . 29 . 28 . 28 . 27 . 28 . 27
Jonathan . 37 . 36 . 42 . 43 . 41 . 43 . 41 . 40 . 40
McIntosh . 25 . 27 . 38 . 37 . 35 . 28 . 28 . 28 . 31
Northern Spy .44 .41 .41 .40 .41 .43 .40 .42 .41
R. I. Greening . 51 . 51 . 51 . 47 . 47 . 54 . 54 . 54 . 52
Stark . 33 . 37 . 35 . 35 . 42 . 39 . 37 . 34 . 36
Stayman . 56 . 53 . 55 . 53 . 55 . 54 . 53 . 51 . 54
Tolman Sweet . O9 .10 .11 .12 . 11 .10 .10 . 10 . 10
Wagener . 45 . 42 . 37 . 37 . 38 . 44 . 38 . 37 . 40
Wealthy .35 .38 .48 .47 .39 . 45 . 39 .40 . 41
Winter Banana .18 . 22 . 21 . 21 . 22 . 22 . 22 . 22 . 21
Wolf River . 45 . 46 . 42 . 49 . 48 . 48 . 48 . 48 . 45

.verage . 34 . 35 . 36 . 36 . 36 . 36 . 36 . 36

1 /

— Each datum represents the average of two determinations.

20.

Soluble Solids Percent of Apple Sauce

TABLE V

 

 

Storage Temperature

 

 

 

 

Variety - 5° F 32° F 70° F 85° F
49 84 42 63 70 35 56 77
days days days days days days days days
(Degree Brix)
Baldwin 17 18 18 18 18 18 18 18
Ben Davis 18 18 18 18 17 17 17 17
Caville Black 17 19 19 18 19 18 18 18
Cortland 17 17 17 17 17 17 17 17
Fameuse 17 18 18 18 18 18 18 18
Golden Delicious 17 17 17 17 17 17 17 17
Grimes Golden 17 16 16 16 16 16 16 16
jonathan 17 17 17 17 17 16 16 16
McIntosh 17 18 18 18 18 18 18 18
Northern Spy 17 18 18 18 18 17 17 17
R. I. Greening 17 18 19 19 19 18 18 18
Stark 18 18 18 18 18 18 18 18
Stayman 17 17 18 17 18 18 17 17
Tolman Sweet 17 17 17 17 17 17 17 17
Wagener 18 18 18 18 18 18 18 18
Wealthy 17 18 18 18 18 l8 18 18
Winter Banana 18 18 18 l8 18 18 18 18
Wolf River 17 17 17 18 18 18 18 18

 

 

21.

22.

showed the least amounts of tin residue, while R. I. Greening, Stark and

Wolf River contained the greatest amounts. No tin was found in the frozen

samples. The amount of tin found in the canned sauce was dependent upon

the time and temperature of storage. Sauces stored at 32°F for 125 days

contained 3. 3 to 10. 2 mg tin per 100 g sauce, at 70°F for 125 days, 5. 0 to

12. 9 mg per 100 g sauce, and at 85°F for 89 days, 4. 8 to 13. 7 mg tin per

100 g sauce (Table VI). The tin present in the apple sauce was probably

due to detinning of the can. Kohn _e_t at: (16) reported that detinning was due

to excessive amount of air in the head space. This could be controlled by

either reducing the head space to a minimum or by closing under conditions

which will remove most of the head space air. Since, in this study, no

precautions were taken to decrease the amount of head space air, the above
results could be expected. It was also noted that there was a detinning line
at the apple sauce level with pronounced darkening of the sauce in those lots
stored at 85°F. No significant relationship was found between the amount

of tin in the apple sauce and the amount of caproic acid formed. The corre-

lation coefficient was . 360.

Acetaldehyde

There was no correlation between acetaldehyde and off flavor develop-

ment of canned apple sauce (r = .190) (Table VII). The small differences

in the amounts found were probably due to varietal differences.

 

TABLE VI

Tin Content of Canned Apple Sauce

 

_ r;-
—_ ——:“___

 

 

 

 

 

 

Variety 32° F Storage Terggegature 85° F Varietal
126 days 125 days 89 days Average
mg/IOO gram s.l_/ ‘
Baldwin 6. 0 8. 7 9. 0 7. 9
Ben Davis 7. 2 8. 0 9. 1 8. l
Caville Black 5. 6 6. 0 5. 0 5. 5
Cortland 7. 0 6. 5 7. 2 6. 9
F ameuse 4. 5 5. 0 4. 8 4. 8
Golden Delicious 9. 0 7. 3 8. 6 8. 3
Erimes Golden 9. 5 9. 6 9. 6 9. 6
mathan 6. 0 6. 9 6. 8 6. 6
’cIntosh 6. 0 9. 0 8. 5 7. 8
irthern Spy 7. 5 7. 8 7. 7 7. 6
I. Greening 9. 0 10. 0 10. 3 9. 8
rk 8.6 11.7 11.5 10.6
Iman 5. 0 7. 9 7. 4 6. 8
nan Sweet . 5. 0 . 6. 5 6. 8 6. 1
ener 4. 8 5. O 4. 8' 4. 8
thy 4. 9 5. 2 5. 0 5. 0
r Banana 3. 3 5. 0 4. 5 4. 3
{iver 10.2 12.9 13.7 12.3
rage 6. 2 7. 7 7. 8
1 / f f

— Each datum represents average of two determinations.

Ammonia N and Amide N

 

Little or no ammonia nitrogen was found in the apple sauce. Small
quantities of amide nitrogen were found present in apple sauce, as shown
in Table VII. Also, it can be seen that only small variation exists between

variety samples.

24.

TABLE VII

Acetaldehyde and Amide N Content of Canned Apple Sauce

 

 

 

 

 

 

 

 

 

Acetaldehyde Amide N
Variety Stored at 85°F $161766 at 85°F
34 days 67 days 40 days
mg/IOO gramsl/ mg/lOO grams

Baldwin 0. 09 0. 07 1. 5
Ben Davis 0. 04 0. 07 1. 3
Caville Black 0. 04 0. 09 1. 5
Cortland 0. O7 0. 07 1. 4
F ameuse 0. 09 0. 09 0. 9
Golden Delicious 0. 04 O. 04 1. 7
Grimes Golden 0. 04 0. O7 0. 6
Jonathan 0. 09 0. 09 1. 6
McIntosh O. 10 0. O7 1. 3
Northern Spy 0. 07 O. 04 1. 4
R. I. Greening 0. 04 0. 04 1. 4
Stark 0. 04 0. 07 1. 3
Stayman 0. 08 0. 04 1. 0
Tolman Sweet 0. 10 0. 09 0. 5
Wagener 0. 09 0. 10 1. 7
Wealthy 0. 09 0. 10 1. 1
Winter Banana 0. 10 0. 10 1. 5
Wolf River 0. 09 0. 09 1. 6

Average 0. 072 0. 072 l. 3

 

-1-/ Each datum represents the average of duplicate determinations.

26.

SUMMARY AND CONCLUSIONS

The purpose of this study was to evaluate the effects of time and tem-
perature on the off flavor development in canned apple sauce produced from
eighteen Michigan grown commercial apple varieties. The off flavor com-
ponent, which was isolated by a carefully standardized steam distillation
procedure was identified as n- caproic acid with paper chromatography.
N—caproic acid was found to develop as a function of time and temperature.
Sauces stored at 32°F contained similar amounts of caproic acid after 84
days of storage as those stored at 70°F for 42 days, or those stored at
85°F for 35 days. The caproic acid formation increased up to 63 and 56
days of storage at 70 and 85°F, respectively, with continued storage show-
ing very little increase in the formation of this component. Considerable
variation in caproic acid content was found between sauces from various
varieties of apples used, with Ben Davis having the greatest amount, and
Tolman Sweet the least amount.

It was concluded that tin and caproic acid content play a part in the
off flavor and odor, but this is not the only factor, since sauces stored at
32° and 70°F show comparable amounts of tin and caproic acid, yet do not
have the pronounced undesirable off flavor characteristics of the sauce

stored at 85°F. At the present time no explanation can be given for this

27.

development. The increase in tin content was probably due to corrosion of

the can promoted by the relatively large head space present in canned apple
sauce (13) which induced corrosion. There was considerable variation between
the varieties as far as consistency, viscosity, soluble solids, total acidity,

pH, tin content, and amide nitrogen, but in general there was very little
change within the same variety during storage, and no odOrous association

was apparent between these factors and the development of caproic acid.

10.

ll.

12.

28.

BIBLIOGRAPHY

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March 16, 1959.

. United States Standards for Grades of Canned Apple Sauce

 

Effective September 18, 1950.

Block, R. J. , E. L. Darrum and G. Zweig. A Manual of Paper Chromo-
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evaluation of apple sauce fortified with essence and citric acid. Food
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. Canning Trade Almanac. Pub. Canning Trade Almanac, Baltimore, Md.

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Child, A. M. , and R. Brand. Culinary quality of apple varieties grown
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. Consumption of Food in United States. Agr. Mkt. Service, U. S. D. A.

Agr. Handbook No. 62, 913-17. 1957.

Crocker, E. C. The nature of flavor, U. S. Egg and Poultry Magazine
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Cruess, W. V. Commercial Fruit and Vegetable Products. 4th Ed. ,
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195-197. 1958.

Dryden, E. C. , and C. H. Hills. Consumer preference studies on apple
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Handbook of Chemistry and Physics. 38th Ed. , Chemical Rubber Publish-
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Huelin, F. E. Volatile products of apples. Australian Jour. Sc. Res.,
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29.

13: Joslyn, N. A. Methods in Food Analysis. Academic Press, New York 10,
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14. , and J. J. Davids. Acetaldehyde and alcohol in raw or under-
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15. Kertesz, Z. 1., and J. D. Laconti. Factors determining the consistency
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16. Kohn, G. G. , and J. E. Fix. Effects of packing procedure on container
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17. Mattick, L. R., J. C. Moyer and R. S. Shallenberg. Volatile acidic flavor
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19. . Volatile compounds produced by apples. IL Alcohols and
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APPENDIX TABLE

Caproic Acid Production in Canned Apple Sauce

 

 

r— _-
T‘ ‘:-'_

Storage Temperature

 

Variety -5°F 32°F 70°F 85°F

 

 

 

49 84 42 63 70 35 56 77
days days days days days days days days

 

mg caproic acid/ 100 gr.

Baldwin 2.8 6.6 7.2 11.4 11.6 8.1 16.0 15.8
3.0 6.8 7.7 11.9 12.2 9.0 15 8 15.9
2.8 6.5 7.5 11.7 12.1 9 2 15.1 15.5
Ben Davis 3.0 8.7 5 7 12.4 12.7 8. 9 17.6 18. 1
3.0 9.0 5. 12.6 13. 5 9.0 18 0 17. 8
3.0 9.0 6. 1 12.4 12.9 8.6 18 1 18.0
Caville Black 2. 8 6. 6 ‘ 6. 3 7. 5 8. 5 7. 8 l3. 9 13 8
2. 7 6. 8 6. 5 8. 0 8. 5 7. 3 13. 7 14. 6
2.6 6.1 6.5 7.9 8.7 7 7 13.7 19 2
Cortland 3. 4 7. 7 6 6 11. 9 12. 4 8. 8 16. 9 17. 4
3.6 7. 9 6. 5 12.2 12.3 8.4 17.3 16.6
3.5 7 7 6.8 11.5 12.6 8.6 17.3 17 3
Fameuse 3 9 11.4 6. 8 9 0 9.6 8.0 11.6 12.1
3.6 11.1 6.7 8 8 9.5 9.0 12.3 12.8
3 8 11.1 6.8 8 9 9.9 8.5 11.8 12.5
Golden Delicious 3 2 1 . 6 6. 6 9. 0 9. 5 6. 5 14. 7 14. 3
3.2 11.1 6 5 9.3 9.7 5.8 14.6 14.7
3.2 10.3 6 8 9 5 9.7 6.6 14.9 14.4
Grimes Golden 3. 9 8 9 6 1 11. 6 11. 6 5. 8 15. 0 15 5
4.1 8.9 5 11.3 11.7 6.7 15.5 15.8
3.8 8 7 51 11.5 11.6 6.3 15.2 15 8
Jonathan 3.9 8.2 5.9 10 1 10.6 5.9 16.4 18 4
4. 1 8. l 5. 8 10 9 10. 7 6. 7 l6. 4 l6. 2
3.8 8.7 5. 9 0 3 10.7 6.1 16.9 16.5
McIntosh 3. 5 7. 8 6. 5 10. 3 12. 3 8. 6 15. 3 15. 3
3.6 7.6 6.5 10.8 12.4 8.9 15.8 16.3
3.6 7.8 6.5 10.4 12.4 8.8 15.3 15.8

11 ._ _ 24.215“.

APPENDIX TABLE CONT' D

 

 

Storage Temperature

 

-5° F 32° F 70° F 85°F
49 84 42 63 70 35 56
days days days days days days days

Variety

 

mg caproic acid/100 gr.

Northern Spy 3. 6 7. 7 9. 4 ll. 4 ll. 9 9. 5 13. 7
3. 5 7.4 9.6 11.6 12.2 8.7 14.4
3.6 7.8 9.0 11.4 12.3 9 0 14.9
R. I. Greening 3. 0 5. 9 8. 5 13. 0 13. 5 11. 2 13 6
3. 2 6. 0 8. 5 13. 6 13. 7 11 3 13. 2
3.1 5. 7 9. 2 12. 8 14. 0 11. 7 13 3
Stark 2. 4 6. 4 6 5 11. 7 12. 5 9 2 15. 3
2. 9 6.1 6. 8 12. 1 12. 4 9. 3 14. 7
2.5 6.0 7 1 11.4 12.5 9.2 15.0
Stayman 3. 1 6. 3 7. 8 11. 8 12. 0 8. 5 17. 2
3.2 6.5 7.3 11.6 12.2 7.9 16.8
3.1 6.4 6.7 11.5 12 4 8.2 17.1
Tolman Sweet 2. 7 7. 7 2. 9 6. 0 7. 0 2. 8 9. 9
2.7 8.0 3.1 6.0 7.8 2.8 9.6
2.7 7.8 2.7 6.6 7.8 3.0 9.2
Wagener 2. 7 7. 5 4. 5 8. 4 8.1 6. 6 11. 8
2.7 7.5 4.1 8.3 9.4 7.0 11.7
2.6 7.2 4.2 8.4 9.4 6.5 11.6
Wealthy 3 0 9.7 7 5 11 7 12.2 11 4 17.7
3.0 10.1 8.7 11 3 11 9 11.7 16 5
3 1 9.6 8.8 11.9 12 3 11.6 15.6
Winter Banana 2. 7 7. 2 5. 8 6. 0 6. 5 6. 6 10. 8
2.4 7.3 5.4 5.6 7.1 6.8 11.8
2.4 7.1 5.6 5.8 7.1 6.6 11.3
Wolf River 2. 7 6. 4 8.1 12. 3 12.2 9. 2 l6. 4
2. 8 6. 5 8.2 11.7 12. 8 9.2 16.8
2. 5 6. 4 8.8 12.2 12.4 9.5 16.4

 

 

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