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7906 Stannous / Official Monographs NF 35

Analysis: Compare the Standard solution and the Sam- IDENTIFICATION

ple solution. • A.
Acceptance criteria: Any color in the Sample solution is Analysis: Examine under a microscope, using a mixture
not more intense than that in the Standard solution of glycerin and water (1:1) as a mounting agent.
(50 µg/g). Acceptance criteria: It appears either as angular poly-
hedral granules of irregular sizes with diameters ranging
SPECIFIC TESTS from 2–23 µm, or as rounded or spheroidal granules of
• APPEARANCE OF SOLUTION irregular sizes with diameters ranging from 25–35 µm.
Standard stock solution: Pipet 30.0 mL of ferric chlo- The central hilum consists of a distinct cavity or two- to
ride CS, 30.0 mL of cobaltous chloride CS, and 24.0 mL five-rayed cleft, and there are no concentric striations.
of cupric sulfate CS into a 100-mL volumetric flask. Di- Between orthogonally oriented polarizing plates or
lute with 1% (w/v) hydrochloric acid to volume. prisms, the starch granules show a distinct black cross
Standard solution: Dilute 1.0 mL of the Standard stock intersecting at the hilum.
solution with 1% (w/v) hydrochloric acid to 100 mL. • B.
Sample solution: Dissolve 10.0 g of Stannous Chloride Sample solution: 20 mg/mL in water
in dilute hydrochloric acid solution, and dilute with di- Analysis: Boil for 1 min, and cool.
lute hydrochloric acid solution to 20 mL. Acceptance criteria: A thin, cloudy mucilage is formed.
Acceptance criteria: The Sample solution is clear and • C.
colorless, or if not, not more intensely colored than the Sample solution: 1 mL of the mucilage obtained in
Standard solution. Identification test B
• SUBSTANCES NOT PRECIPITATED BY THIOACETAMIDE Analysis: Add 0.05 mL of iodine and potassium iodide
Sample solution: Dissolve 1.0 g of Stannous Chloride in TS 2 to the Sample solution.
dilute hydrochloric acid solution, and dilute with the Acceptance criteria: An orange-red to dark blue color
same acid to 30 mL. Heat to boiling. Add 30 mL of thi- is produced, which disappears upon heating.
oacetamide TS, and boil for 15 min to produce Solution
A. Filter 5 mL of Solution A, and heat the filtrate to boil- IMPURITIES
ing. Add 5 mL of thioacetamide TS, and boil for 15 • RESIDUE ON IGNITION 〈281〉
min. If a precipitate is formed, add the remainder of Sample: 1.0 g
Solution A to the mixture to produce Solution A1. Add Acceptance criteria: NMT 0.6%
10 mL of thioacetamide TS, and boil. Repeat the series • LIMIT OF IRON
of operations from “Filter 5 mL” until a precipitate is no Standard iron stock solution A: Equivalent to 10 µg/
longer formed on addition of thioacetamide TS to the mL of iron prepared as directed in Iron 〈241〉
filtrate obtained from the 5 mL of Solution A (Solution Standard iron stock solution B: 1 µg/mL of iron from
A1, Solution A2, and so on, respectively). If no precipi- Standard iron stock solution A in water
tate is formed, or if no more precipitate is formed, [NOTE—Prepare immediately before use.]
combine the solution obtained with the remainder of Standard iron solution: Transfer 10 mL of Standard iron
Solution A (Solution A1, Solution A2, and so on, respec- stock solution B to a test tube, and add 2 mL of citric
tively), filter, and wash the precipitate with 10 mL of acid solution (2 in 10) and 0.1 mL of thioglycolic acid.
water. Heat the filtrate until the resulting vapor no Add 10 N ammonium hydroxide until the solution is
longer turns a moistened piece of lead acetate test pa- distinctly alkaline to litmus, and dilute with water to
per blackish-gray. Allow to cool, and dilute with water 20 mL.
to 50 mL. [NOTE—Keep a portion for the Limit of Iron Sample solution: Shake 1.5 g of Corn Starch with
test.] 15 mL of 2 N hydrochloric acid, and filter. Transfer
Analysis: Evaporate 25 mL of the Sample solution to 10 mL of the filtrate to a test tube, add 2 mL of citric
dryness, and ignite at 600°. acid solution (2 in 10), and 0.1 mL of thioglycolic acid.
Acceptance criteria: The residue weighs NMT 1 mg Add 10 N ammonium hydroxide until the solution is
(0.2%). distinctly alkaline to litmus, and dilute with water to
20 mL.
ADDITIONAL REQUIREMENTS Acceptance criteria: After 5 min, any pink color in the
• PACKAGING AND STORAGE: Preserve in well-closed contain- Sample solution is not more intense than that in the
ers. No storage requirements specified. Standard iron solution, corresponding to a limit of
NF Monographs

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.

Corn Starch Bromophenol blue indicator solution: 0.2 mg/mL of
Portions of the monograph text that are national USP text, bromophenol blue in dilute alcohol. Filter if necessary.
and are not part of the harmonized text, are marked with Hydrogen peroxide solution: Dilute 30% hydrogen
symbols (◆◆) to specify this fact. peroxide with water to obtain a 3% solution. Just
before use, add 3 drops of Bromophenol blue indicator
.

DEFINITION solution, and neutralize to a violet-blue endpoint with

Corn Starch consists of the starch granules separated from 0.01 N sodium hydroxide. Do not exceed the endpoint.
the mature grain of corn [Zea mays L. (Fam. Gramineae)].

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NF 35 Official Monographs / Starch 7907

Apparatus: See Figure 1. 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
Figure 1 the disappearance of the starch–iodine color. Perform a
In this test, the sulfur dioxide is released from the sam- blank determination, and make any necessary correc-
ple in a boiling acid medium and is removed by a tion. Each mL of 0.002 N sodium thiosulfate is equiva-
stream of carbon dioxide. The separated gas is col- lent to 34 µg of oxidant, calculated as hydrogen
lected in a dilute hydrogen peroxide solution where peroxide.
the sulfur dioxide is oxidized to sulfuric acid and ti- Acceptance criteria: NMT 1.4 mL of 0.002 N sodium
trated with standard alkali. The apparatus consists es- thiosulfate is required (20 ppm, calculated as H2O2).
sentially of a 500-mL three-neck, round-bottom boiling
flask, A; a separatory funnel, B, having a capacity of SPECIFIC TESTS
100 mL or greater; a gas inlet tube of sufficient length • MICROBIAL ENUMERATION TESTS 〈61〉 and TESTS FOR SPECI-
FIED MICROORGANISMS 〈62〉: The total aerobic microbial
to permit introduction of the carbon dioxide within
2.5 cm of the bottom of the boiling flask; a reflux con- count does not exceed 103 cfu/g; the total combined
.

denser, C, having a jacket length of 200 mm, and a molds and yeasts count does not exceed 102 cfu/g; and
.

delivery tube, E, connecting the upper end of the re- it meets the requirements of the test for the absence of
flux condenser to the bottom of a receiving test tube, Escherichia coli. ◆Where it is intended for use in preparing
.

D. Apply a thin film of stopcock grease to the sealing Absorbable Dusting Powder, it also meets the require-
surfaces of all of the joints except the joint between ments of the tests for absence of Staphylococcus aureus
the separatory funnel and the boiling flask, and clamp and Pseudomonas aeruginosa.◆
the joints to ensure tightness. • LOSS ON DRYING 〈731〉
Sample: 25.0 g of Corn Starch Sample: 1 g
Analysis: Add 150 mL of water to the boiling flask. Analysis: Dry the Sample at 130° for 90 min.
Close the stopcock of the separatory funnel, and begin Acceptance criteria: NMT 15.0%
• PH 〈791〉

NF Monographs
the flow of carbon dioxide at a rate of 100 ± 5 mL/min
through the Apparatus. Start the condenser coolant Sample solution: Prepare a slurry by weighing 5.0 g of
flow. Add 10 mL of Hydrogen peroxide solution to a re- Corn Starch, transferring to a suitable nonmetallic con-
ceiving test tube. After 15 min, without interrupting the tainer, and adding 25.0 mL of freshly boiled and cooled
flow of carbon dioxide, remove the separatory funnel water.
from the boiling flask, and transfer the Sample into the Analysis: Agitate continuously at a moderate rate for 1
boiling flask with the aid of 100 mL of water. Apply min. Stop the agitation, and allow to stand for 15 min.
stopcock grease to the outer joint of the separatory fun- Determine the pH to the nearest 0.1 unit.
nel, and replace the separatory funnel in the boiling Acceptance criteria: 4.0–7.0
flask. Close the stopcock of the separatory funnel, and ADDITIONAL REQUIREMENTS
add 80 mL of 2 N hydrochloric acid to the separatory • ◆PACKAGING AND STORAGE: Preserve in well-closed con-
funnel. Open the stopcock of the separatory funnel to
.

tainers. No storage requirements specified.◆

permit the hydrochloric acid solution to flow into the • ◆LABELING: Where Corn Starch is intended for use in pre-
boiling flask, guarding against the escape of sulfur diox-
.

paring Absorbable Dusting Powder, it is so labeled, and

ide into the separatory funnel by closing the stopcock the label states that it must be subjected to further pro-
before the last few mL of hydrochloric acid drain out. cessing during the preparation of Absorbable Dusting
Boil the mixture for 1 h. Remove the receiving test Powder.◆
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.
Accessed from 10.6.1.1 by brunswick20 on Tue Feb 21 06:27:10 EST 2017

7908 Starch / Official Monographs NF 35

Acceptance criteria: A violet color develops within 5

min due to the presence of hydroxypropyl groups
.

Hydroxypropyl Corn Starch (starch ether).

ASSAY
• PROCEDURE FOR HYDROXYPROPYL GROUPS
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-
For the Amylose derivative, m is about 300–1000. peat the operation two more times. If poor dispersibility
or slow filtration is observed, use refrigerated carbon
DEFINITION dioxide-free water for the washing operation. Dry the
Hydroxypropyl Corn Starch is partially substituted 2-hydrox- washed starch for NLT 4 h in vacuum at 30 ± 5°. Deter-
ypropylether obtained from corn starch by a chemical mine the moisture content (B) on 5 g of the washed
modification of etherification with propylene oxide. In ad- and dried starch following the Loss on Drying test.
dition, this starch may be partially hydrolyzed using acids Weigh 12.0 mg of the washed and dried starch in a
or enzymes to obtain thinned starch. It contains NLT 5-mm NMR tube. Add 0.75 mL of deuterium oxide and
2.0% and NMT 7.0% of hydroxypropyl groups on the 0.1 mL of Deuterium chloride solution. Cap the tube,
dried basis. mix, and place it in a boiling water bath until a clear
IDENTIFICATION solution is obtained. [NOTE—This may take 3 min to 1
• A. PROCEDURE h.] When a clear solution is obtained, allow to cool to
Analysis: Examine under a microscope, using NLT 20× room temperature. Dry the exterior of the tube, and
magnification and a mixture of glycerin and water (1:1) weigh to the nearest 0.1 mg. Add 0.05 mL of Internal
as a mounting agent. standard solution, and weigh to the nearest 0.1 mg. De-
Acceptance criteria: It presents either as angular poly- termine the mass of the Internal standard solution
hedral granules of irregular sizes with diameters of 2–23 added. Mix thoroughly.
µm, or as rounded or spheroidal granules of irregular Nuclear magnetic resonance spectrometry
sizes with diameters of 25–35 µm. The central hilum (See Nuclear Magnetic Resonance Spectroscopy 〈761〉,
consists of a distinct cavity or 2- to 5-rayed cleft, and Quantitative Applications.)
there are no concentric striations. Between crossed nicol Apparatus: FT-NMR spectrometer at minimum
prisms, the Hydroxypropyl Corn Starch granules show a 300 MHz
distinct black cross intersecting at the hilum. Acquisition of 1H NMR spectra: The following param-
.

• B. PROCEDURE eters may be used.

Sample solution: Suspend 1 g of Hydroxypropyl Corn Sweep width: 8 ppm (about −1.0 to +7 ppm)
Starch in 50 mL of water, boil for 1 min, and cool. Irradiation frequency offset: None
Acceptance criteria: A translucent or clear mucilage is Time domain: NLT 64 K
formed. Pulse width: 90 degree
• C. PROCEDURE Pulse delay: 10 s
Analysis: To 1 mL of the Sample solution obtained in Dummy scans: 0
Identification test B add 0.05 mL of iodine and potas- Number of scans: 8
sium iodide TS 2. Use the CH3 signal of the internal standard for shift
Acceptance criteria: An orange-red to dark blue color referencing. Set the shift of the peak of the singlet to
is produced, which disappears upon heating. 0 ppm. Record the FID signal.
• D. PROCEDURE Analysis
Ninhydrin solution: Dissolve 3 g of ninhydrin in Samples: Internal standard solution and Sample solution
NF Monographs

100 mL of a 45.5-g/L solution of sodium metabisulfite. Call the integration sub-routine after phase corrections
Diluted sulfuric acid: 98 g/L of H2SO4 and baseline correction between −0.5 and +6 ppm.
Sample: 100 mg of Hydroxypropyl Corn Starch Measure the peak areas of the doublet from the methyl
Analysis: Transfer the Sample to a 100-mL volumetric groups of the hydroxypropyl function at +1.2 ppm
flask, and add 12.5 mL of Diluted sulfuric acid. Place the (A2), and of the methyl groups at 0 ppm of the inter-
flask in a water bath, and heat until the Sample is dis- nal standard (A1) without 13C-satellites.
.

solved. Cool, and dilute with water to 100 mL. [CAU- Measure the signal coming from the 3 protons of the
TION—When sulfuric acid is miscible with water, it pro-
methyl group in the hydroxypropyl function.
duces intense heat.] Calculate the content of hydroxypropyl groups as a per-
Pipet 1 mL of this solution to a glass-stoppered, 25-mL centage (w/w, dried basis):
graduated test tube and, with the tube immersed in Result = (N × A2/A1) × (Ci × Wi/W) × (Mr2/Mr1) × [100/
cold water, add drop-wise 8 mL of sulfuric acid. Mix (100 − B)] × 100
well, and place the tube in a boiling water bath for
exactly 3 min. Immediately transfer the tube to an ice N = numerical value representing the 3 methyl
bath until the solution is chilled. Add 0.6 mL of groups in the internal standard (sodium
Ninhydrin solution, carefully allowing the reagent to 3-trimethylsilyl-1-propane sulfonate), 3
run down the walls of the test tube. Immediately A2 = area of the methyl groups of hydroxypropyl in
shake the tube well, and place it in a water bath at Hydroxypropyl Corn Starch
25° for 100 min. Dilute with sulfuric acid to 25 mL A1 = area of the methyl groups in the internal
[CAUTION—Use sulfuric acid cautiously.], and mix by standard (sodium 3-trimethylsilyl-1-propane
inverting the tube several times. Do not shake. sulfonate)
Ci = concentration of the internal standard in the
Internal standard solution (mg/g)

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Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.