Stage 6 Harmonization
Official August 1, 2015 Starch 1
.
Acceptance criteria: After 5 min, any pink color in the
Sample solution is not more intense than that in the
Rice Starch
Standard iron solution, corresponding to a limit of
10 ppm of iron.
• L
IMIT
OF
S
ULFUR
D
IOXIDE
Add the following:
Carbon dioxide: Use carbon dioxide, with a flow reg-
ulator that will maintain a flow of 100 ±
■
.
5
■1S (NF33)
■
.
Portions of this monograph that are national USP text, and
mL/min.
are not part of the harmonized text, are marked with
■
.
■1S (NF33)
symbols (
◆
.
◆
) to specify this fact.
■1S (NF33)
Hydrogen peroxide solution: Dilute 30% hydrogen
peroxide with water to obtain a 3% solution. Just
DEFINITION
before use, add 3 drops of
■
.
bromophenol blue TS,
Rice Starch is obtained from the caryopsis of Oryza sativa
■1S (NF33)
and neutralize to a violet-blue endpoint with
L.
■
.
0.1 N
■1S (NF33)
sodium hydroxide. Do not exceed the
endpoint.
IDENTIFICATION
Apparatus: See Figure 1.
Change to read:
• A
.
P
ROCEDURE
Analysis: Examine under a microscope, using NLT 20×
magnification and using a mixture of glycerin and
water (1:1) as a mounting agent.
Acceptance criteria:
■
.
It presents polyhedral, simple
grains 1–10 µm, mostly 4–6 µm in size. These simple
grains often gather in ellipsoidal, compound grains
50–100 µm in diameter. The granules have a poorly
visible central hilum and there are no concentric stria-
tions. Between orthogonally orientated polarising
plates or prisms, the starch granules show a distinct
black cross intersecting at the hilum.
■1S (NF33)
• B
.
P
ROCEDURE
Sample solution: 20 mg/mL in water
Analysis: Boil for 1 min, and cool.
Acceptance criteria: A thin, cloudy mucilage is
formed.
• C
.
P
ROCEDURE
Sample solution: 1 mL of the mucilage obtained in
Identification test B
Analysis: Add 0.05 mL of iodine and potassium iodide
TS 2 to the Sample solution.
Acceptance criteria: An orange-red to dark blue color
is produced, which disappears upon heating.
Figure 1
IMPURITIES
In this test, the sulfur dioxide is released from the
sample in a boiling acid medium and is removed by
Change to read:
a stream of carbon dioxide. The separated gas is col-
lected in a dilute hydrogen peroxide solution where
Inorganic Impurities
the sulfur dioxide is oxidized to sulfuric acid and ti-
• R
ESIDUE
ON
I
GNITION
〈281〉: NMT 0.6%, determined on a
trated with standard alkali. The apparatus consists es-
1.0-g sample
sentially of a 500-mL three-neck, round-bottom boil-
• L
IMIT
OF
I
RON
ing flask, A; a separatory funnel, B, with a capacity of
Standard iron stock solution A: Equivalent to 10 µg/
100 mL or greater; a gas inlet tube of sufficient
mL of iron prepared as directed in Iron 〈241〉
length to permit introduction of the carbon dioxide
Standard iron stock solution B: 1 µg/mL of iron from
within 2.5 cm of the bottom of the boiling flask; a
Standard iron stock solution A in water
reflux condenser, C, with a jacket length of 200 mm;
[N
OTE
—Prepare immediately before use.]
and a delivery tube, E, connecting the upper end of
Standard iron solution: Transfer 10 mL of Standard
the reflux condenser to the bottom of a receiving
iron stock solution B to a test tube, and add 2 mL of
test tube, D. Apply a thin film of stopcock grease to
citric acid solution (2 in 10) and 0.1 mL of thioglycolic
the sealing surfaces of all of the joints except the
acid. Add 10 N ammonium hydroxide until the solu-
joint between the separatory funnel and the boiling
tion is distinctly alkaline to litmus, and dilute with
flask, and clamp the joints to ensure tightness.
water to 20 mL.
Sample: 25.0 g of Rice Starch
Sample solution: Shake 1.5 g of Rice Starch with
Analysis: Add 150 mL of water to the boiling flask.
15 mL of 2 N hydrochloric acid, and filter. Transfer
Close the stopcock of the separatory funnel, and begin
10 mL of the filtrate to a test tube, and add 2 mL of
the flow of carbon dioxide at a rate of 100 ± 5
citric acid solution (2 in 10) and 0.1 mL of thioglycolic
mL/min through the Apparatus. Start the condenser
acid. Add 10 N ammonium hydroxide until the solu-
coolant flow. Add 10 mL of Hydrogen peroxide solution
tion is distinctly alkaline to litmus, and dilute with
to a receiving test tube. After 15 min, without inter-
water to 20 mL.
rupting the flow of carbon dioxide, remove the sepa-
2014 The United States Pharmacopeial Convention All Rights Reserved.
Stage 6 Harmonization
2 Starch Official August 1, 2015
ratory funnel from the boiling flask, and transfer the form a blank determination, and make any necessary
Sample into the boiling flask with the aid of 100 mL of correction. Each mL of 0.002 N sodium thiosulfate is
water. Apply stopcock grease to the outer joint of the equivalent to 34 µg of oxidant, calculated as hydrogen
separatory funnel, and replace the separatory funnel in peroxide.
the boiling flask. Close the stopcock of the separatory Acceptance criteria: NMT 1.4 mL of 0.002 N sodium
funnel, and add 80 mL of 2 N hydrochloric acid to the thiosulfate is required [20 ppm, calculated as hydro-
separatory funnel. Open the stopcock of the separa- gen peroxide (H
2
O
2
)]
tory funnel to permit the hydrochloric acid solution to
SPECIFIC TESTS
flow into the boiling flask, guarding against the escape
of sulfur dioxide into the separatory funnel by closing
the stopcock before the last few mL of hydrochloric
Change to read:
acid drain out. Boil the mixture for 1 h. Remove the
receiving test tube, and transfer its contents to a
•
■
.
■1S (NF33)
M
ICROBIAL
E
NUMERATION
T
ESTS
〈61〉 and T
ESTS
FOR
200-mL wide-necked, conical flask. Rinse the receiving
S
PECIFIED
M
ICROORGANISMS
〈62〉: The total aerobic micro-
test tube with a small portion of water, add the rins-
bial count does not exceed 10
3
.
cfu/g; the total combined
ing to the 200-mL conical flask, and mix. Heat on a
molds and yeasts count does not exceed 10
2
.
cfu/g; and
water bath for 15 min, and allow to cool.
it meets the requirements of the test for the absence of
Add 0.1 mL of
■
.
bromophenol blue TS,
■1S (NF33)
and ti-
Escherichia coli.
■
.
■1S (NF33)
trate the contents with 0.1 N sodium hydroxide VS
• L
OSS
ON
D
RYING
〈731〉
until the color changes from yellow to violet-blue.
Sample: 1 g
Perform a blank determination, and make any neces-
Analysis: Dry the Sample at 130° for 90 min.
sary correction (see Titrimetry 〈541〉).
Acceptance criteria: NMT 15.0%
Calculate the content, in ppm, of sulfur dioxide in the
Sample taken:
Change to read:
Result = (V × N × F)/W × 1000
•
P
H 〈791〉
■
.
■1S (NF33)
V = volume of titrant consumed (mL)
Sample solution: Prepare a slurry by weighing 5.0 g of
N = normality of the titrant
Rice Starch, transferring to a suitable nonmetallic con-
F = milliequivalent weight of sulfur dioxide, 32.03
tainer, and adding 25.0 mL of freshly boiled and
W = weight of the Sample (g)
cooled water.
Acceptance criteria: NMT 50 ppm
Analysis: Agitate continuously at a moderate rate for 1
• L
IMIT
OF
O
XIDIZING
S
UBSTANCES
min. Stop the agitation, and allow to stand for 15 min.
Sample solution: Transfer 4.0 g to a glass-stoppered,
Determine the pH to the nearest 0.1 unit.
125-mL conical flask, and add 50.0 mL of water. Insert
■
.
Acceptance criteria: 5.0–8.0
■1S (NF33)
the stopper, and swirl for 5 min. Transfer to a glass-
stoppered, 50-mL centrifuge tube, and centrifuge to
ADDITIONAL REQUIREMENTS
clarify. Transfer 30.0 mL of the clear supernatant to a
•
◆
.
P
ACKAGING
AND
S
TORAGE
: Preserve in well-closed con-
glass-stoppered, 125-mL conical flask. Add 1 mL of
tainers. No storage requirements specified.
◆
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.
Analysis: Titrate with 0.002 N sodium thiosulfate VS
to the disappearance of the starch–iodine color. Per-
2014 The United States Pharmacopeial Convention All Rights Reserved.
