Accessed from 10.6.1.
1 by brunswick20 on Tue Feb 21 06:27:10 EST 2017
7906 Stannous / Official Monographs
Analysis: Compare the Standard solution and the Sam-
ple solution.
Acceptance criteria: Any color in the Sample solution is
not more intense than that in the Standard solution
(50 µg/g).
SPECIFIC TESTS
• APPEARANCE OF SOLUTION
Standard stock solution: Pipet 30.0 mL of ferric chlo-
ride CS, 30.0 mL of cobaltous chloride CS, and 24.0 mL
of cupric sulfate CS into a 100-mL volumetric flask. Di-
lute with 1% (w/v) hydrochloric acid to volume.
Standard solution: Dilute 1.0 mL of the Standard stock
solution with 1% (w/v) hydrochloric acid to 100 mL.
Sample solution: Dissolve 10.0 g of Stannous Chloride
in dilute hydrochloric acid solution, and dilute with di-
lute hydrochloric acid solution to 20 mL.
Acceptance criteria: The Sample solution is clear and
colorless, or if not, not more intensely colored than the
Standard solution.
• SUBSTANCES NOT PRECIPITATED BY THIOACETAMIDE
Sample solution: Dissolve 1.0 g of Stannous Chloride in
dilute hydrochloric acid solution, and dilute with the
same acid to 30 mL. Heat to boiling. Add 30 mL of thi-
oacetamide TS, and boil for 15 min to produce Solution
A. Filter 5 mL of Solution A, and heat the filtrate to boil-
ing. Add 5 mL of thioacetamide TS, and boil for 15
min. If a precipitate is formed, add the remainder of
Solution A to the mixture to produce Solution A1. Add
10 mL of thioacetamide TS, and boil. Repeat the series
of operations from “Filter 5 mL” until a precipitate is no
longer formed on addition of thioacetamide TS to the
filtrate obtained from the 5 mL of Solution A (Solution
A1, Solution A2, and so on, respectively). If no precipi-
tate is formed, or if no more precipitate is formed,
combine the solution obtained with the remainder of
Solution A (Solution A1, Solution A2, and so on, respec-
tively), filter, and wash the precipitate with 10 mL of
water. Heat the filtrate until the resulting vapor no
longer turns a moistened piece of lead acetate test pa-
per blackish-gray. Allow to cool, and dilute with water
to 50 mL. [NOTE—Keep a portion for the Limit of Iron
test.]
Analysis: Evaporate 25 mL of the Sample solution to
dryness, and ignite at 600°.
Acceptance criteria: The residue weighs NMT 1 mg
(0.2%).
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in well-closed contain-
ers. No storage requirements specified.
NF Monographs
.
Corn Starch
Portions of the monograph text that are national USP text,
and are not part of the harmonized text, are marked with
symbols (◆◆) to specify this fact.
.
DEFINITION
Corn Starch consists of the starch granules separated from
the mature grain of corn [Zea mays L. (Fam. Gramineae)].
Official from null
Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
NF 35
IDENTIFICATION
• A.
Analysis: Examine under a microscope, using a mixture
of glycerin and water (1:1) as a mounting agent.
Acceptance criteria: It appears either as angular poly-
hedral granules of irregular sizes with diameters ranging
from 2–23 µm, or as rounded or spheroidal granules of
irregular sizes with diameters ranging from 25–35 µm.
The central hilum consists of a distinct cavity or two- to
five-rayed cleft, and there are no concentric striations.
Between orthogonally oriented polarizing plates or
prisms, the starch granules show a distinct black cross
intersecting at the hilum.
• B.
Sample solution: 20 mg/mL in water
Analysis: Boil for 1 min, and cool.
Acceptance criteria: A thin, cloudy mucilage is formed.
• C.
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.
IMPURITIES
• RESIDUE ON IGNITION 〈281〉
Sample: 1.0 g
Acceptance criteria: NMT 0.6%
• LIMIT OF IRON
Standard iron stock solution A: Equivalent to 10 µg/
mL of iron prepared as directed in Iron 〈241〉
Standard iron stock solution B: 1 µg/mL of iron from
Standard iron stock solution A in water
[NOTE—Prepare immediately before use.]
Standard iron solution: Transfer 10 mL of Standard iron
stock solution B to a test tube, and add 2 mL of citric
acid solution (2 in 10) and 0.1 mL of thioglycolic acid.
Add 10 N ammonium hydroxide until the solution is
distinctly alkaline to litmus, and dilute with water to
20 mL.
Sample solution: Shake 1.5 g of Corn Starch with
15 mL of 2 N hydrochloric acid, and filter. Transfer
10 mL of the filtrate to a test tube, add 2 mL of citric
acid solution (2 in 10), and 0.1 mL of thioglycolic acid.
Add 10 N ammonium hydroxide until the solution is
distinctly alkaline to litmus, and dilute with water to
20 mL.
Acceptance criteria: After 5 min, any pink color in the
Sample solution is not more intense than that in the
Standard iron solution, corresponding to a limit of
10 ppm of iron.
• LIMIT OF SULFUR DIOXIDE
Carbon dioxide: Use carbon dioxide, with a flow regu-
lator that will maintain a flow of 100 ± 10 mL/min.
Bromophenol blue indicator solution: 0.2 mg/mL of
bromophenol blue in dilute alcohol. Filter if necessary.
Hydrogen peroxide solution: Dilute 30% hydrogen
peroxide with water to obtain a 3% solution. Just
before use, add 3 drops of Bromophenol blue indicator
solution, and neutralize to a violet-blue endpoint with
0.01 N sodium hydroxide. Do not exceed the endpoint.
Accessed from 10.6.1.1 by brunswick20 on Tue Feb 21 06:27:10 EST 2017
NF 35
Apparatus: See Figure 1.
Figure 1
In this test, the sulfur dioxide is released from the sam-
ple in a boiling acid medium and is removed by a
stream of carbon dioxide. The separated gas is col-
lected in a dilute hydrogen peroxide solution where
the sulfur dioxide is oxidized to sulfuric acid and ti-
trated with standard alkali. The apparatus consists es-
sentially of a 500-mL three-neck, round-bottom boiling
flask, A; a separatory funnel, B, having a capacity of
100 mL or greater; a gas inlet tube of sufficient length
to permit introduction of the carbon dioxide within
2.5 cm of the bottom of the boiling flask; a reflux con-
denser, C, having a jacket length of 200 mm, and a
delivery tube, E, connecting the upper end of the re-
flux condenser to the bottom of a receiving test tube,
D. Apply a thin film of stopcock grease to the sealing
surfaces of all of the joints except the joint between
the separatory funnel and the boiling flask, and clamp
the joints to ensure tightness.
Sample: 25.0 g of Corn Starch
Analysis: Add 150 mL of water to the boiling flask.
Close the stopcock of the separatory funnel, and begin
the flow of carbon dioxide at a rate of 100 ± 5 mL/min
through the Apparatus. Start the condenser coolant
flow. Add 10 mL of Hydrogen peroxide solution to a re-
ceiving test tube. After 15 min, without interrupting the
flow of carbon dioxide, remove the separatory funnel
from the boiling flask, and transfer the Sample into the
boiling flask with the aid of 100 mL of water. Apply
stopcock grease to the outer joint of the separatory fun-
nel, and replace the separatory funnel in the boiling
flask. Close the stopcock of the separatory funnel, and
add 80 mL of 2 N hydrochloric acid to the separatory
funnel. Open the stopcock of the separatory funnel to
permit the hydrochloric acid solution to flow into the
boiling flask, guarding against the escape of sulfur diox-
ide into the separatory funnel by closing the stopcock
before the last few mL of hydrochloric acid drain out.
Boil the mixture for 1 h. Remove the receiving test
tube, and transfer its contents to a 200-mL wide-
necked, conical flask. Rinse the receiving test tube with
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Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Starch 7907
a small portion of water, add the rinsing to the 200-mL
conical flask, and mix. Heat on a water bath for 15
min, and allow to cool.
Add 0.1 mL of Bromophenol blue indicator solution, and
titrate the contents with 0.1 N sodium hydroxide VS
until the color changes from yellow to violet-blue. Per-
form a blank determination, and make any necessary
correction (see Titrimetry 〈541〉).
Calculate the content, in ppm, of sulfur dioxide in the
Sample taken:
Result = (V × N × F)/W × 1000
V = volume of titrant consumed (mL)
N = normality of the titrant
F = milliequivalent weight of sulfur dioxide, 32.03
W = weight of the Sample (g)
Acceptance criteria: NMT 50 ppm
• LIMIT OF OXIDIZING SUBSTANCES
Sample solution: Transfer 4.0 g 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 conical flask. Add 1 mL of gla-
cial acetic acid and 0.5–1.0 g of potassium iodide. In-
sert 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. Perform a
blank determination, and make any necessary correc-
tion. Each mL of 0.002 N sodium thiosulfate is equiva-
lent to 34 µg of oxidant, calculated as hydrogen
peroxide.
Acceptance criteria: NMT 1.4 mL of 0.002 N sodium
thiosulfate is required (20 ppm, calculated as H2O2).
SPECIFIC TESTS
• MICROBIAL ENUMERATION TESTS 〈61〉 and TESTS FOR SPECI-
FIED MICROORGANISMS 〈62〉: The total aerobic microbial
count does not exceed 103 cfu/g; the total combined
.
molds and yeasts count does not exceed 102 cfu/g; and
.
it meets the requirements of the test for the absence of
Escherichia coli. ◆Where it is intended for use in preparing
.
Absorbable Dusting Powder, it also meets the require-
ments of the tests for absence of Staphylococcus aureus
and Pseudomonas aeruginosa.◆
• LOSS ON DRYING 〈731〉
Sample: 1 g
Analysis: Dry the Sample at 130° for 90 min.
Acceptance criteria: NMT 15.0%
• PH 〈791〉
NF Monographs
Sample solution: Prepare a slurry by weighing 5.0 g of
Corn Starch, transferring to a suitable nonmetallic con-
tainer, and adding 25.0 mL of freshly boiled and cooled
water.
Analysis: Agitate continuously at a moderate rate for 1
min. Stop the agitation, and allow to stand for 15 min.
Determine the pH to the nearest 0.1 unit.
Acceptance criteria: 4.0–7.0
ADDITIONAL REQUIREMENTS
• ◆PACKAGING AND STORAGE: Preserve in well-closed con-
.
tainers. No storage requirements specified.◆
• ◆LABELING: Where Corn Starch is intended for use in pre-
.
paring Absorbable Dusting Powder, it is so labeled, and
the label states that it must be subjected to further pro-
cessing during the preparation of Absorbable Dusting
Powder.◆
 Accessed from 10.6.1.1 by brunswick20 on Tue Feb 21 06:27:10 EST 2017
7908 Starch / Official Monographs
.
Hydroxypropyl Corn Starch
ASSAY
• PROCEDURE FOR HYDROXYPROPYL GROUPS
For the Amylose derivative, m is about 300–1000.
DEFINITION
Hydroxypropyl Corn Starch is partially substituted 2-hydrox-
ypropylether obtained from corn starch by a chemical
modification of etherification with propylene oxide. In ad-
dition, this starch may be partially hydrolyzed using acids
or enzymes to obtain thinned starch. It contains NLT
2.0% and NMT 7.0% of hydroxypropyl groups on the
dried basis.
IDENTIFICATION
• A. PROCEDURE
Analysis: Examine under a microscope, using NLT 20×
magnification and a mixture of glycerin and water (1:1)
as a mounting agent.
Acceptance criteria: It presents either as angular poly-
hedral granules of irregular sizes with diameters of 2–23
µm, or as rounded or spheroidal granules of irregular
sizes with diameters of 25–35 µm. The central hilum
consists of a distinct cavity or 2- to 5-rayed cleft, and
there are no concentric striations. Between crossed nicol
prisms, the Hydroxypropyl Corn Starch granules show a
distinct black cross intersecting at the hilum.
• B. PROCEDURE
Sample solution: Suspend 1 g of Hydroxypropyl Corn
Starch in 50 mL of water, boil for 1 min, and cool.
Acceptance criteria: A translucent or clear mucilage is
formed.
• C. PROCEDURE
Analysis: To 1 mL of the Sample solution obtained in
Identification test B add 0.05 mL of iodine and potas-
sium iodide TS 2.
Acceptance criteria: An orange-red to dark blue color
is produced, which disappears upon heating.
• D. PROCEDURE
Ninhydrin solution: Dissolve 3 g of ninhydrin in
NF Monographs
100 mL of a 45.5-g/L solution of sodium metabisulfite.
Diluted sulfuric acid: 98 g/L of H2SO4
Sample: 100 mg of Hydroxypropyl Corn Starch
Analysis: Transfer the Sample to a 100-mL volumetric
flask, and add 12.5 mL of Diluted sulfuric acid. Place the
flask in a water bath, and heat until the Sample is dis-
solved. Cool, and dilute with water to 100 mL. [CAU-
TION—When sulfuric acid is miscible with water, it pro-
duces intense heat.]
Pipet 1 mL of this solution to a glass-stoppered, 25-mL
graduated test tube and, with the tube immersed in
cold water, add drop-wise 8 mL of sulfuric acid. Mix
well, and place the tube in a boiling water bath for
exactly 3 min. Immediately transfer the tube to an ice
bath until the solution is chilled. Add 0.6 mL of
Ninhydrin solution, carefully allowing the reagent to
run down the walls of the test tube. Immediately
shake the tube well, and place it in a water bath at
25° for 100 min. Dilute with sulfuric acid to 25 mL
[CAUTION—Use sulfuric acid cautiously.], and mix by
inverting the tube several times. Do not shake.
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NF 35
Acceptance criteria: A violet color develops within 5
min due to the presence of hydroxypropyl groups
(starch ether).
Deuterium chloride solution: Dilute 1 mL of deuterium
chloride (38% w/w) with 5 mL of deuterium oxide.
Internal standard solution: Disperse 50.0 mg of so-
dium 3-trimethylsilyl-1-propane sulfonate in about 5 g
of deuterium oxide, weighed to the nearest 0.1 mg.
Store in a sealed bottle.
Sample solution: Disperse 20 g of Hydroxypropyl Corn
Starch in 200.0 mL of carbon dioxide-free water at
room temperature. Agitate for 15 min, and filter. Re-
peat the operation two more times. If poor dispersibility
or slow filtration is observed, use refrigerated carbon
dioxide-free water for the washing operation. Dry the
washed starch for NLT 4 h in vacuum at 30 ± 5°. Deter-
mine the moisture content (B) on 5 g of the washed
and dried starch following the Loss on Drying test.
Weigh 12.0 mg of the washed and dried starch in a
5-mm NMR tube. Add 0.75 mL of deuterium oxide and
0.1 mL of Deuterium chloride solution. Cap the tube,
mix, and place it in a boiling water bath until a clear
solution is obtained. [NOTE—This may take 3 min to 1
h.] When a clear solution is obtained, allow to cool to
room temperature. Dry the exterior of the tube, and
weigh to the nearest 0.1 mg. Add 0.05 mL of Internal
standard solution, and weigh to the nearest 0.1 mg. De-
termine the mass of the Internal standard solution
added. Mix thoroughly.
Nuclear magnetic resonance spectrometry
(See Nuclear Magnetic Resonance Spectroscopy 〈761〉,
Quantitative Applications.)
Apparatus: FT-NMR spectrometer at minimum
300 MHz
Acquisition of 1H NMR spectra: The following param-
.
eters may be used.
Sweep width: 8 ppm (about −1.0 to +7 ppm)
Irradiation frequency offset: None
Time domain: NLT 64 K
Pulse width: 90 degree
Pulse delay: 10 s
Dummy scans: 0
Number of scans: 8
Use the CH3 signal of the internal standard for shift
referencing. Set the shift of the peak of the singlet to
0 ppm. Record the FID signal.
Analysis
Samples: Internal standard solution and Sample solution
Call the integration sub-routine after phase corrections
and baseline correction between −0.5 and +6 ppm.
Measure the peak areas of the doublet from the methyl
groups of the hydroxypropyl function at +1.2 ppm
(A2), and of the methyl groups at 0 ppm of the inter-
nal standard (A1) without 13C-satellites.
.
Measure the signal coming from the 3 protons of the
methyl group in the hydroxypropyl function.
Calculate the content of hydroxypropyl groups as a per-
centage (w/w, dried basis):
Result = (N × A2/A1) × (Ci × Wi/W) × (Mr2/Mr1) × [100/
(100 − B)] × 100
N = numerical value representing the 3 methyl
groups in the internal standard (sodium
3-trimethylsilyl-1-propane sulfonate), 3
A2 = area of the methyl groups of hydroxypropyl in
Hydroxypropyl Corn Starch
A1 = area of the methyl groups in the internal
standard (sodium 3-trimethylsilyl-1-propane
sulfonate)
Ci = concentration of the internal standard in the
Internal standard solution (mg/g)