Accessed from 128.83.63.

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USP 35

Official Monographs / Aurothioglucose 2273

atropine sulfate [(C 17H23NO3)2 H2SO4 H2O] in the portion of

Tablets taken by the formula:
(694.85 / 676.83)(W / 10)(RU / RS)
in which 694.85 and 676.83 are the molecular weights of atropine sulfate monohydrate and anhydrous atropine sulfate, respectively; W is the weight, in mg, of USP Atropine Sulfate RS
in the Standard preparation; and RU and RS are as defined
therein.

Activated Attapulgite
.

Activated Attapulgite is a highly heat-treated,

processed, native magnesium aluminum silicate.
Packaging and storagePreserve in well-closed containers.
IdentificationActivated Attapulgite responds to the Identification test for Colloidal Activated Attapulgite, the characteristic
peak, however, being much less intense.
Loss on drying 731Dry it at 105 to constant weight: it
loses not more than 4.0% of its weight.
Loss on ignition 733When ignited at 1000 for 1 hour, it
loses between 4.0% and 12.0% of its weight.
Volatile matterWhen ignited at 600 for 1 hour, it loses
between 3.0% and 7.5% of its weight on the dried basis.
Powder finenessProceed as directed in the test for Powder
fineness under Colloidal Activated Attapulgite. The dr y weight of
the residue is not more than 0.10% of the weight of the specimen taken.
Acid-soluble matterBoil 2.0 g with 100 mL of 0.2 N hydrochloric acid for 5 minutes, and cool. Add water to adjust the
volume to 100 mL, and filter. Evaporate 50 mL of the filtrate so
obtained to dr yness, and ignite the residue at 600 : not more
than 0.25 g is found (25%).
Other requirementsIt meets the requirements of the tests
for Microbial limits, pH, Carbonate, Arsenic and Lead, and Adsorptive capacity under Colloidal Activated Attapulgite.

Colloidal Activated Attapulgite

.

Colloidal Activated Attapulgite is a purified native magnesium aluminum silicate.

Packaging and storagePreserve in well-closed containers.
IdentificationAdd 2 g in small portions to 100 mL of water,
with vigorous agitation. Allow to stand for at least 12 hours to
ensure complete hydration. Place 2 mL of the resulting mixture
on a suitable glass slide, and allow to air-dr y at room temperature to produce a uniform film. Place the slide in a vacuum
desiccator over a free sur face of ethylene glycol. Evacuate the
desiccator, and close the stopcock so that the ethylene glycol
saturates the desiccator chamber. Allow to stand for 12 hours.
Record the X-ray diffraction pattern (see X-Ray Diffraction
941), and calculate the d values: several peaks are obser ved;
the characteristic peak corresponds to a d value between 10.3
and 10.7 Angstrom units.
Microbial enumeration tests 61 and Tests for specified
microorganisms 62It meets the requirements of the test
for absence of Escherichia coli.
pH 791Disperse 1.0 g in 10 mL of carbon dioxide-free
water, and mix: the pH of the mixed dispersion so obtained is
between 7.0 and 9.5.
Loss on drying 731Dry it at 105 to constant weight: it
loses between 5.0% and 17.0% of its weight.

Loss on ignition 733When ignited at 1000 for 1 hour, it

loses between 17.0% and 27.0% of its weight.
Volatile matterWhen ignited at 600 for 1 hour, it loses
between 7.5% and 12.5% of its weight on the dried basis.
Powder finenessAdd 50 g to 450 mL of water containing
5 g of sodium pyrophosphate, and stir for 10 minutes. Pour the
resulting dispersion slowly through a No. 325 standard sieve
(see Particle Size Distribution Estimation by Analytical Sieving
786), and carefully wash the residue until clean. Dr y the residue at 105 to constant weight: the dr y weight of the residue
so obtained is not more than 0.30% of the weight of the specimen taken.
Acid-soluble matterBoil 2.0 g with 100 mL of 0.2 N hydrochloric acid for 5 minutes, and cool. Add water to adjust the
volume to 100 mL, and filter. Evaporate 50 mL of the filtrate so
obtained to dr yness, and ignite the residue at 600 : not more
than 0.15 g is found (15%).
CarbonateMix 1.0 g with 15 mL of 0.5 N sulfuric acid: no
effervescence occurs.
Arsenic and LeadTo 5.0 g add 50 mL of 1 N nitric acid,
and boil for 30 minutes, adding 1 N nitric acid at times to
maintain the volume. Filter into a 100-mL volumetric flask,
wash the filter with water, and dilute the combined filtrate and
washings with water to volume.
ArsenicDetermine the arsenic in the solution by atomic absorption spectrometry (see Spectrophotometry and Light-scattering 851), using a graphite furnace to volatilize the arsenic, as
directed by the manufacturer of the instrument used, and
measuring the absorbance at 189.0 nm against a standard: not
more than 2 ppm is found.
LeadDetermine the lead in the solution by atomic absorption spectrometry (see Spectrophotometry and Light-scattering
851), using a graphite furnace to volatilize the lead, as directed by the manufacturer of the instrument used, and measuring the absorbance at 283.3 nm against a standard: not more
than 0.001% is found.
Adsorptive capacityTo 10 mL of a 1 in 10 suspension of
the specimen in water add 80 mL of methylene blue solution (1
in 1000), and shake. Add 10 mL of barium chloride solution (1
in 50), and shake. Allow to stand for 15 minutes. T ransfer 40
mL of the supernatant to a 50-mL centrifuge tube, and centrifuge. To 5 mL of the clear supernatant add 495 mL of water,
and mix: the color of the solution so obtained is not deeper
than that of a solution containing 1.5 g of methylene blue per
mL.

Aurothioglucose
.

C6H11AuO5S 392.18
Gold, (1-thio- D-glucopyranosato)-.
(1-Thio-D-glucopyranosato)gold [12192-57-3].

Aurothioglucose contains not less than 95.0

percent and not more than 105.0 per cent of
C6H11AuO5S, calculated on the dried basis. It is
stabilized by the addition of a small amount of
Sodium Acetate.
Packaging and storagePreserve in tight, light-resistant
containers. Store at room temperature.
USP Reference standards 11
USP Aurothioglucose RS

Official from May 1, 2012

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

Accessed from 128.83.63.20 by nEwp0rt1 on Mon Nov 21 22:45:44 EST 2011

2274 Aurothioglucose / Official Monographs

Identification
A: Dissolve a suitable quantity in water to obtain a solution
containing 4 mg per mL. Apply 10 L of this solution and 10
L of an aqueous Standard solution of USP Aurothioglucose RS
containing 4 mg per mL to a suitable thin-layer chromatographic glass microfilament sheet (see Chromatography 621)
impregnated with silicic acid and a suitable fluorescing substance. Allow the spots to dr y, and develop the chromatogram
in a solvent system consisting of a mixture of n-propyl alcohol,
water, and ethyl acetate (3:3:1) until the solvent front has
moved about three-fourths of the length of the plate. Remove
the sheet from the developing chamber, mark the solvent front,
and allow the solvent to evaporate. Locate the spots on the
plate by examination under short-wavelength UV light: the RF
value of the principal spot obtained from the solution under
test corresponds to that obtained from the Standard solution.
B: To a portion of the filtrate obtained in the Assay add
barium chloride TS: a heavy, white precipitate is formed.
Specific rotation 781S: between +65 and +75 .
Test solution: 10 mg per mL, in water.
Loss on drying 731Dry it over phosphorus pentoxide for
24 hours: it loses not more than 1.0% of its weight.
AssayAccurately weigh about 1 g of Aurothioglucose, and
dissolve in 100 mL of water in a 300-mL Kjeldahl flask. Slowly
add 10 mL of nitric acid, and when the reaction has subsided,
boil the mixture for 5 minutes. Filter, wash well the separated
gold with hot water, dr y, and ignite to constant weight. The
weight of the gold so obtained, multiplied by 1.991, represents
the weight of C 6H11AuO5S in the portion of Aurothioglucose
taken.

Aurothioglucose Injectable Suspension

.

Aurothioglucose Injectable Suspension is a sterile suspension of Aurothioglucose in a suitable

vegetable oil. It contains not less than 90.0 percent and not more than 110.0 per cent of the
labeled amount of C 6H11AuO5S. It may contain
suitable thickening agents.
Packaging and storagePreserve in single-dose or in multiple-dose containers, preferably of T ype I glass. Protect from
light.
USP Reference standards 11
USP Aurothioglucose RS
IdentificationTransfer a volume of Injectable Suspension,
equivalent to about 200 mg of aurothioglucose, to a centrifuge
separator containing 20 mL of ethyl acetate and 50 mL of
water. Shake the mixture thoroughly, and centrifuge until the
liquid phases have been clearly separated. W ithdraw the lower,
aqueous phase, and filter, discarding the first 10 mL of the
filtrate. Collect the filtrate in a glass-stoppered vessel, and proceed as directed in Identification test A under Aurothioglucose,
beginning with apply 10 L of this solution.
Bacterial endotoxins 85It contains not more than 7.14
USP Endotoxin Units per mg of aurothioglucose.
Sterility 71It meets the requirements.
Other requirementsIt meets the requirements under Injections 1.
AssayTransfer with a pipet, calibrated to contain rather than
to deliver, an accurately measured volume of Injectable Suspension, equivalent to about 200 mg of aurothioglucose, to a
beaker containing 400 mL of acetone. W ash the pipet into the
beaker with a small quantity of acetone, mix, allow the solids to
settle, and decant the supernatant through a filter. W ash the
solids with another 400-mL portion of acetone, and repeat the
decantation. Transfer the solids to the filter with the aid of ace-

USP 35
tone, then transfer the filter and its contents to a short-necked,
300-mL Kjeldahl flask, add 5 mL of water, and proceed as directed in the Assay under Gold Sodium Thiomalate, beginning
with add 20 mL of nitric acid. The weight of gold so obtained, multiplied by 1.991, represents the weight of
C6H11AuO5S in the portion of Injectable Suspension taken.

Avobenzone
.

C20H22O3 310.40
1,3-Propanedione, 1-[4-(1,1-dimethylethyl)phenyl]-3-(4-methoxyphenyl)-.
1-(p-tert-Butylphenyl)-3-(p-methoxyphenyl)-1,3-propanedione
[70356-09-1].

Avobenzone contains not less than 95.0 percent and not more than 105.0 per cent of
C20H22O3, calculated on the dried basis.
Packaging and storagePreserve in tight, light-resistant
containers.
USP Reference standards 11
USP Avobenzone RS
Identification
A: Infrared Absorption 197K.
B: Ultraviolet Absorption 197U
Solution: 5 g per mL.
Medium: alcohol.
Absorptivities at 360 nm do not differ by more than 3.0%.
Melting range, Class I 741: between 81 and 86 .
Loss on drying 731Dry it in vacuum at 70 for 4 hours: it
loses not more than 0.5% of its weight.
Chromatographic purity
Test solutionProceed as directed for Assay preparation in
the Assay.
Chromatographic system (see Chromatography 621)Proceed as directed in the Assay.
ProcedureInject a volume (about 1 L) of Test solution into
the chromatograph, record the chromatogram, and measure
the peak responses. Calculate the per centage of each impurity
in the portion of A vobenzone taken by the formula:
100(rI / rS)
in which rI is the response of each individual peak, other than
the avobenzone peak, in the chromatogram of the Test solution;
and rS is the sum of the responses of all of the peaks in the
chromatogram of the Test solution: not more than 3.0% of any
individual impurity is found, and the sum of all of the impurities
is not more than 4.5%.
Assay
Standard preparationDilute an accurately measured quantity of USP A vobenzone RS in acetone, and dilute quantitatively,
and stepwise if necessar y, with acetone to obtain a solution
having a known concentration of about 50 mg per mL.
Assay preparationTransfer about 500 mg of A vobenzone,
accurately weighed, to a 10-mL volumetric flask, dilute with
acetone to volume, and mix.
Chromatographic system (see Chromatography 621)The
gas chromatograph is equipped with a flame-ionization detector
and a 0.32-mm 25-m fused silica capillar y column coated
with phase G1. The column temperature is maintained at about

Official from May 1, 2012

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