260 FLORIDA STATE HORTICULTURAL SOCIETY, 1973

IMPROVED METHOD FOR THE EXTRACTION OF PECTIN1

Joseph M. G. Huang Company, Anaheim, California. IER were ob
tained from Rohm and Haas Company of Phila
N L Industries, Inc.
delphia.
Research and Development Department General Procedure for the Hydrochloric Acid
P.O. Box 420 Extraction of Pectin. A mixture of 60g of dried
Hightstown, New Jersey 08520 lemon, orange, or grapefruit peel and 3600g of
deionized water was stirred and heated to 85°C.
Abstract. Methods of extracting pectin from Concentrated HC1 was added drop wise to adjust
various citrus peels were studied using hydro the pH to 1.6. More HC1 was.added if necessary
chloric acid, organic acids, and their salts and ion- when pH was rechecked after 15 minutes. The
exchange resins (IER) as extractant. A novel mixture was continuously stirred and maintained
method based on IER and mineral acid adjustment at 85 °C for one hour. Hot water was added to
of proper pH has given increased yields of pectin restore 3600g net weight at the end of heating
with quality maintained at the highest levels. The period and 60g of Celite 503 filter aid was then
quality factor of the extracted pectin is strongly added to the slurry. The mixture was filtered on
dependent upon the pH of the extracting solution 9 inch Buchner funnel precoated with 96g of
and a maximum exists at pH of 1.6 for a pre Celite. The filtrate was cooled to room tempera
ferred sulfonated resin. ture and 3600 ml of isopropanol were added to
precipitate the pectin. The precipitate was
Introduction drained and squeezed on a muslin cloth and puri
fied by breaking the solid into 1200 ml of 60%
A long list of various agents has been re by weight isopropanol, containing 10 ml of 5%
ported for the extraction of pectin from plant NaHC03. Purification was repeated in 500 ml of
tissues. (1) Extraction with hot water is the isopropanol and the pectin was dried in a vacuum
simplest and oldest method for removing the oven at 45 °C overnight. The weighed pectin was
pectic substances. The most commonly used ma ground to pass 20 mesh in a Wily Mill.
terials are mineral acids including sulfuric, General Procedure for the IER Extraction of
hydrochloric, and phosphoric acids. (2). Many Pectin. Sixty grams of orange peel, 1800g of
organic acids and their salts such as oxalic acid water and 18g of the IER were heated to 85°C
(3), ammonium oxalate (4), tartaric acid (5), with constant stirring. Water was added occa
polyphosphates (6), and many others (7) have sionally to maintain constant volume, and the
also been used. Meyers and Rouse (8) reported
heating and stirring were maintained at this
the use of a H-Zeolite IER for the extraction of
temperature for 1 hour. The solid materials were
pectin. A very low yield of pectin obtained from
filtered with the aid of Celite and worked up as
dried orange peel was reported (9) using Zeocarb described above.
as extractant at 85-90°C. Double extraction at
85-88°C for one hour using a cationic resin for Results and Discussion
the extraction of pectin from apple pomace has
been reported to give higher yields and better gel Following the general procedure for the
strength of the product. (10) IER have been hydrochloric acid (HCi) extraction method, a
extensively used in the purification and fractiona- 28.7%, 22.9%, and 19.S% yield of purified pectins
tion of pectin. (11) were obtained based upon the dried citrus peel
of lemon, grapefruit, arid orange respectively.
The peel to water ratio was held at 1:60, and
Materials and Methods
the extraction was carried at 85° C for 1 hour
Materials with pH of 1.6 throughout the period.
Six IER samples ranging from strongly acidic
Dried lemon, orange, and grapefruit peels
to weakly basic and mixed type were evaluated.
were received from Anaheim Citrus Products
Early stages of the investigation were confined
to orange peel and Amberlite 120+ (a sulfonated
lThe author wishes to express his sincere gratitude to polystyrene resin) until the optimum timing, the
Messrs. R. J. Berndlmaier and R. A. Wilgus for the ex
perimental assistance.
amount of water and resin, temperature and con-
 BRADDOCK & KESTERSON: DRIED CITRUS JUICE SACS 261

centration were established. Selection of the at the final pH adjustment of 1.6 prior to filtra
resin was then based on these same parameters tion. Moreover, since the yields and gel grades
to ensure the right conditions for each batch. have all been improved considerably, the quality
The best procedure and resin selected were then factor which determines the overall quality of the
adopted for comparison of the yields with that product has to be enhanced.
of mineral acid method. The yields of pectins The gel strength and the yields of the ex
were 25.0%, 21.5%, and 20.5% for Amberlite tracted pectin varied with the acidic concentra
IR-120+ resin extraction of lemon, grapefruit, tion have been observed. The resin—HC1 extrac
and orange peel respectively at a comparable tion method was broadened to include a wide pH
experimental conditions. range and to involve many resins. It then became
Gel grade (12) comparison of the resin ex evident that a final pH adjustment between 1.35-
tracted pactins with those of HC1 extracted 1.60 gave better yields and gel grades than either
indicated that the latter have higher gel grades higher or lower pH's. The quality factor of the
than those of resin extracted. The HC1 extracted extracted pectin is strongly dependent upon the
pectin from lemon peel, for example, has a grade pH of the solution. A pH—quality factor curve
of 176 in, comparison with 106 from IR-120+ shows a maximum of pH 1.6 using Amberlite
resin and 119 from MB-1 resin. The ester con IR-120 -f as extractant.
tents of the resin extracted pectins were found
to be ten-fold higher than those of acid extracted. Literature Cited
A second series of extractions were studied using 1. Z. I. Kertesz. 1958. The pectic substances. Interscience
the previous extraction procedure except the pH Publishers, Inc.
2. G. L. Baker and E. E. Karr. 1946. Fruit Prod. J.
of the slurry at the end was adjusted with cone. 25:292.
3. M. Manabe, et. al. 1966. Chem. Abstracts. 65:10786e.
HC1 to 1.6-2.6. The results of these extractions 4. P. B. Myers, et. al. 1934. Univ. Delaware Agr. Expt.
indicate that the yields obtained were better, and Sta. Bull. No. 187.
5. B. S. Lewandowska. 1965. Chem. Abstract. 60:2179.
the gel grades of these produces were improved. 6. R. M. McCready, et. al. 1947. Fruit Prod. J. 27:36.
7. M. A. Joslyn and H. Deuel. 1963. J. Food Sci. 28 :65.
For example, a grade of 187, 186, and 159 and a 8. P. B. Myers and A. H. Rouse. 1943. U.S. Pat. 2,323,484.
yield of 30.0%, 27.5%, and 23.3% were found for 9. M. Bailly. 1956. Chem. Abstract. 50:3670e.
10. P. Banov, et. al. 1958. Chem. Abstract. 53.9507i.
pectins extracted from lemon, grapefruit, and 11. K. Steiner, H. Neukom, and H. Deuel. 1958. Chem.
Abstract. 52:18230.
orange peels respectively using IR-120 + resin 12. Final Report of IFT. 1959. Food Technology. 13:496.

DRIED CITRUS JUICE SACS FOR THE FOOD AND

BEVERAGE INDUSTRIES

R. J. Braddock and J. W. Kesterson mixes, beverage bases, dehydrated puddings, etc.

It also should be possible to use dried juice sacs
IFAS Agricultural Research and Education
to replace the frozen juice sacs currently used in
Center
certain citrus-containing liquid beverages. Since
Lake Alfred
these commodities are natural food products
rather than manufactured additives, they should
Abstract. Finisher pulp from juice processing prove to be valuable food adjuncts for specialty
operations consists primarily of juice vesicles or food processors.
"sacs." These juice sacs may be drum-dried to a
moisture content of less than 10%. Dried juice
Juice sacs (finisher pulp) account for about
sacs have many potential uses in the food and
10 to 20% of the total refuse from citrus juice
beverage industries. Some uses which have been
plants and are considered to be one of the major
proposed include water and fat absorption in
contributors to air pollutants from citrus feed
comminuted meat products, breading mixes for
mill stack gases (2). Some quantities (5000-
fried foods, pie fillings, dehydrated beverage
10,000 lb/yr) of juice sacs are stored frozen in
5-gal containers and primarily sold for use in
Florida Agricultural Experiment Stations Journal Series
No. 5101. beverages containing citrus solids. A brief de-