Accessed from 128.83.63.
20 by nEwp0rt1 on Wed Nov 30 04:14:23 EST 2011
1972 Starch / Official Monographs
IDENTIFICATION
• A.
Corn starch: Polygonal, rounded, or spheroidal granules up
to 35 µm in diameter and usually having a circular or sev-
eral-rayed central cleft
Tapioca starch: Spherical granules with one truncated side,
typically 5–35 µm in diameter and usually having a circular
or several-rayed central cleft
Potato starch: Irregularly shaped, ovoid, or pear-shaped
granules, usually 30–100 µm in size but occasionally exceed-
ing 100 µm; or rounded, 10–35 µm in size. There are occa-
sional compound granules having two to four components.
The ovoid and pear-shaped granules have an eccentric hi-
lum, and the rounded granules have an accentric or slightly
eccentric hilum. All granules show clearly visible concentric
striations.
Wheat starch: Large and small granules, usually 10–60 µm
in diameter. The central hilum and striations are visible or
barely visible.
• B.
Sodium hydroxide solution: 2% (w/w)
Sample: 0.6 g
Analysis: Transfer the Sample to a 25-mL glass vial with a
plastic cap. Add 9.4 g of water, cap, and shake vigorously to
evenly disperse the starch. Add 10 g of the Sodium hydroxide
solution, cap, and shake vigorously for 1 min to create a
smooth mixture. Evaluate within 1 min.
Acceptance criteria: The final solution is translucent to
opaque with a fluid consistency. A yellow tint of the final
solution is acceptable.
• C. A water slurry of the Modified Starch is colored orange-
red to deep blue by iodine TS.
IMPURITIES
• RESIDUE ON IGNITION 〈281〉
Sample: 2.0 ± 0.1 g
Analysis: Proceed as directed in the chapter.
Acceptance criteria: NMT 1.5%
• IRON 〈241〉
Test preparation: Dissolve the residue obtained in the test
for Residue on Ignition in 8 mL of hydrochloric acid with the
aid of gentle heating. Dilute with water to 100 mL in a
volumetric flask, and mix. Dilute 25 mL of this solution with
water to 47 ± 1 mL.
Analysis: Proceed as directed in the chapter.
Acceptance criteria: NMT 20 ppm
• LIMIT OF SULFUR DIOXIDE
Sample: 20.0 ± 0.1 g
Analysis: Mix the Sample with 200 mL of 5% alcohol until a
smooth suspension is obtained, and vacuum-filter through
paper (Whatman No.1 or equivalent). To 100 mL of the
filtrate add 3 mL of starch TS, and titrate with 0.01 N iodine
VS to the first permanent blue color.
Acceptance criteria: NMT 1.7 mL of 0.01 N iodine VS is
consumed, which corresponds to NMT 50 ppm of sulfur di-
oxide being found
• OXIDIZING SUBSTANCES
Sample: 4.0 g
Titrimetric system
Mode: Direct titration
Titrant: 0.002 N sodium thiosulfate VS
Blank: 30.0 mL of water, accurately measured
Endpoint detection: Visual
Analysis: Transfer the Sample to a glass-stoppered, 125-mL
conical flask, and add 50.0 mL of water. Insert the stopper,
and swirl for 5 min. Transfer to a glass-stoppered, 50-mL
centrifuge tube, and centrifuge to clarify. Transfer 30.0 mL
of the clear supernatant to a glass-stoppered, 125-mL coni-
cal flask. Add 1 mL of glacial acetic acid and 0.5–1.0 g of
potassium iodide. Insert the stopper, swirl, and allow to
stand for 25–30 min in the dark. Add 1 mL of starch TS,
and titrate with Titrant to the disappearance of the
starch–iodine color. Perform a blank determination, and
make any necessary correction. Each mL of 0.002 N sodium
Official from May 1, 2012
Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.
NF 30
thiosulfate is equivalent to 34 µg of oxidant, calculated as
hydrogen peroxide.
Acceptance criteria: NMT 12.6 mL of 0.002 N sodium thio-
sulfate is required (180 ppm, calculated as H2O2), which cor-
responds to NMT 0.018% of oxidizing substances
SPECIFIC TESTS
• MICROBIAL ENUMERATION TESTS 〈61〉 and TESTS FOR SPECIFIED
MICROORGANISMS 〈62〉: The total aerobic microbial count
does not exceed 103 cfu/g, and the total combined molds
and yeasts count does not exceed 102 cfu/g. It meets the
requirements of the tests for absence of Salmonella species
and Escherichia coli.
• PH 〈791〉
Sample: 20.0 ± 0.1 g
Analysis: Transfer the Sample to a suitable nonmetallic con-
tainer, and add 100 mL of water to obtain a slurry. Stir
using a magnetic stirrer at a moderate rate for 5 min, and
determine the pH to the nearest 0.1 unit.
Acceptance criteria: 3.0–9.0
• LOSS ON DRYING 〈731〉
Analysis: Dry a sample at 120° for 4 h.
Acceptance criteria
Corn starch and Wheat starch: NMT 15.0%
Tapioca starch: NMT 18.0%
Potato starch: NMT 21.0%
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in well-closed containers.
No storage requirements specified.
.
Pregelatinized Starch
DEFINITION
Pregelatinized Starch is Starch that has been chemically and/or
mechanically processed to rupture all or part of the granules
in the presence of water and subsequently dried. Some types
of Pregelatinized Starch may be modified to render them
compressible and flowable in character.
IDENTIFICATION
• A water slurry of it is colored orange-red to deep blue by
iodine TS.
IMPURITIES
Inorganic Impurities
• RESIDUE ON IGNITION 〈281〉: NMT 0.5%, determined on a 2.0-
g test specimen
• IRON 〈241〉: NMT 20 ppm
Analysis: Dissolve the residue obtained in the test for Resi-
due on Ignition in 8 mL of hydrochloric acid with the aid of
gentle heating, and dilute with water to 100 mL. Dilute 25
mL of this solution with water to 47 mL.
• LIMIT OF SULFUR DIOXIDE
Sample solution: Mix 20 g with 200 mL of a 1 in 5 solution
of anhydrous sodium sulfate, and filter.
Analysis: To 100 mL of the clear filtrate add 3 mL of starch
TS, and titrate with 0.01 N iodine VS to the first permanent
blue color.
Acceptance criteria: NMT 2.7 mL is consumed (80 ppm).
SPECIFIC TESTS
• MICROBIAL ENUMERATION TESTS 〈61〉 and TESTS FOR SPECIFIED
MICROORGANISMS 〈62〉: It meets the requirements of the
tests for absence of Salmonella species and Escherichia coli.
The total aerobic microbial count does not exceed 1000
cfu/g; and the total combined molds and yeasts count does
not exceed 100 cfu/g.
• PH 〈791〉: 4.5–7.0
Prepare a slurry by weighing 10.0 ± 0.1 g in 10 mL of
alcohol and by diluting with water to 100 mL. Agitate con-
tinuously at a moderate rate for 5 min, then cease agitation
Accessed from 128.83.63.20 by nEwp0rt1 on Wed Nov 30 04:14:23 EST 2011

NF 30 Official Monographs / Starch 1973

and immediately potentiometrically determine the pH to

Corn Starch
.

the nearest 0.1 unit.

• LOSS ON DRYING 〈731〉: Dry a sample at 120° for 4 h: it loses
NMT 14.0% of its weight.
• OXIDIZING SUBSTANCES Attributes EP JP USP
Sample: 5 g Definition + + +
Analysis: To the Sample add 20 mL of a mixture of equal Identification A + + +
volumes of methanol and water, then add 1 mL of 6 N ace- Identification B + + +
tic acid, and stir until a homogeneous suspension is ob-
Identification C + + +
tained. Add 0.5 mL of a freshly prepared, saturated solution
of potassium iodide, and allow to stand for 5 min. pH + + +
Acceptance criteria: No distinct blue, brown, or purple Loss on Drying + + +
color is observed. Residue on Ignition + + +
Limit of Iron + + +
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in well-closed containers. Limit of Oxidizing Substances + + +
No storage requirements specified. Limit of Sulfur Dioxide + + +
• LABELING: Label it to indicate the botanical source from
which it was derived. Legend: + will adopt and implement; − will not stipulate
Nonharmonized attributes: Characters, Microbial Enumeration
Tests and Tests for Specified Microorganisms, Labeling, and
Packaging and Storage (USP)
.
Specific local attributes: Foreign matter (EP)
Reagents and reference materials: Each pharmacopeia will
Pregelatinized Modified Starch adapt the text to take account of local reference materials
and reagent specifications.
» Pregelatinized Modified Starch is Modified
Starch that has been chemically or mechanically DEFINITION
processed, or both, to rupture all or part of the Corn Starch consists of the starch granules separated from the
mature grain of corn [Zea mays Linnè (Fam. Gramineae)].
granules to produce a product that swells in cold
water. IDENTIFICATION
• A. PROCEDURE: Examine under a microscope, using NLT 20×
Identification— magnification and using a mixture of glycerin and water
A: Prepare a 2% (w/w) sodium hydroxide solution. Weigh (1:1) as a mounting agent.
0.6 g of Pregelatinized Modified Starch, and transfer to a 25-mL Acceptance criteria: It appears either as angular polyhedral
glass vial with a plastic cap. Add 9.4 g of water, cap, and shake granules of irregular sizes with diameters ranging from 2–23
vigorously to evenly disperse the starch. Add 10 g of 2% NaOH µm, or as rounded or spheroidal granules of irregular sizes
solution, cap, and shake vigorously for 1 minute to create a with diameters ranging from 25–35 µm. The central hilum
smooth mixture. Evaluate within 1 minute. The final solution is consists of a distinct cavity or two- to five-rayed cleft, and
translucent to opaque with a fluid consistency. A yellow tint of there are no concentric striations. Between orthogonally ori-
the final solution is acceptable. ented polarizing plates or prisms, the starch granules show a
B: An aqueous dispersion of Pregelatinized Modified Starch is distinct black cross intersecting at the hilum.
colored orange-red to deep blue by iodine TS. • B. PROCEDURE
Sample solution: 20 mg/mL in water
pH 〈791〉—Wet 10.0 ± 0.1 g of Pregelatinized Modified Starch
Analysis: Boil for 1 min, and cool.
with 10 mL of alcohol, then dilute with water to 300 mL to
Acceptance criteria: A thin, cloudy mucilage is formed.
obtain an aqueous dispersion. Stir continuously at a moderate
• C. PROCEDURE
rate for 5 minutes, and determine the pH to the nearest 0.1
Sample solution: 1 mL of the mucilage obtained in Identifi-
unit: between 3.0 and 9.0.
cation test B
Loss on drying 〈731〉—Dry it at 120° for 4 hours: it loses not Analysis: Add 0.05 mL of iodine and potassium iodide TS 2
more than 15% of its weight. to the Sample solution.
Residue on ignition 〈281〉: not more than 1.5%, a test speci- Acceptance criteria: An orange-red to dark blue color is
men of 2.0 ± 0.1 g being used. produced, which disappears upon heating.
Oxidizing substances—To 5 g of Pregelatinized Modified
Starch add 20 mL of a mixture of methanol and water (1:1), IMPURITIES
then add 1 mL of 6 N acetic acid, and stir until a homogeneous Inorganic Impurities
suspension is obtained. Add 0.5 mL of a freshly prepared satu- • RESIDUE ON IGNITION 〈281〉: NMT 0.6%, determined on a 1.0-
rated solution of potassium iodide, mix, and allow to stand for g sample
5 minutes: no distinct blue, brown, or purple color is observed. • LIMIT OF IRON
Standard iron stock solution A: Equivalent to 10 µg/mL of
Limit of sulfur dioxide—Mix 20.0 ± 0.1 g of Pregelatinized iron prepared as directed under Iron 〈241〉
Modified Starch with 100 mL of 95 percent alcohol, and stir for Standard iron stock solution B: 1 µg/mL of iron from
several minutes to completely wet the starch. Slowly add 100 Standard iron stock solution A in water
mL of water, and stir until a smooth suspension is obtained. [NOTE—Prepare immediately before use.]
Allow the starch mixture to set undisturbed until most of the Standard iron solution: Transfer 10 mL of Standard iron
starch has settled, and filter the aqueous portion through paper stock solution B to a test tube, and add 2 mL of citric acid
(Whatman No. 1 or equivalent). To 100 mL of the clear filtrate solution (2 in 10) and 0.1 mL of thioglycolic acid. Add
add 100 mL of water, and mix. Add 3 mL of starch TS, and 10 N ammonium hydroxide until the solution is distinctly
titrate with 0.01 N iodine VS to the first permanent blue or alkaline to litmus, and dilute with water to 20 mL.
purple color. Not more than 1.7 mL is consumed: not more Sample solution: Shake 1.5 g of Corn Starch with 15 mL
than 0.005% of sulfur dioxide is found. of 2 N hydrochloric acid, and filter. Transfer 10 mL of the
Other requirements—It meets the requirements for Packag- filtrate to a test tube, add 2 mL of citric acid solution (2 in
ing and storage and in the tests for Microbial limits and Iron 10), and 0.1 mL of thioglycolic acid. Add 10 N ammonium
under Modified Starch. hydroxide until the solution is distinctly alkaline to litmus,
and dilute with water to 20 mL.

Official from May 1, 2012

Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.