Accessed from 36.71.237.
98 by belmont7 on Mon Nov 26 09:25:31 EST 2018
866 Chloramphenicol / Official Monographs
contains not less than 90.0 percent and not more
than 130.0 percent of the labeled amount of
C11H12Cl2N2O5.
Packaging and storage—Preserve in tight containers.
USP Reference standards 〈11〉—
USP Chloramphenicol RS
Identification—The retention time of the major peak in
the chromatogram of the Assay preparation corresponds to
that in the chromatogram of the Standard preparation as
obtained in the Assay.
Sterility Tests 〈71〉—It meets the requirements when
tested as directed for Membrane Filtration under Test for Ste-
rility of the Product to be Examined.
pH 〈791〉: between 4.0 and 8.0, when diluted with an
equal volume of water.
Water Determination, Method I 〈921〉: not more than
2.0%.
Assay—
Mobile phase and Chromatographic system—Proceed as di-
rected in the Assay under Chloramphenicol.
Standard preparation—Dissolve an accurately weighed
quantity of USP Chloramphenicol RS in Mobile phase, and
dilute quantitatively, and stepwise if necessary, with Mobile
phase to obtain a solution having a known concentration of
about 100 µg per mL. Filter a portion of this solution
through a 0.5-µm or finer porosity filter, and use the clear
filtrate as the Standard preparation.
Assay preparation—Transfer an accurately measured vol-
ume of Otic Solution, equivalent to about 50 mg of chlor-
amphenicol, to a 100-mL volumetric flask, dilute with Mobile
phase to volume, and mix. Transfer 5.0 mL of the resulting
solution to a 25-mL volumetric flask, dilute with Mobile
phase to volume, and mix. Filter a portion of this solution
through a 0.5-µm or finer porosity filter, and use the clear
USP Monographs
filtrate as the Assay preparation.
Procedure—Proceed as directed for Procedure in the Assay
under Chloramphenicol. Calculate the quantity, in mg, of
C11H12Cl2N2O5 in each mL of the Otic Solution taken by the
formula:
0.5(C / V)(rU / rS)
in which V is the volume, in mL, of Otic Solution taken, and
the other terms are as defined therein.
Chloramphenicol Tablets
.
» Chloramphenicol Tablets contain not less than
90.0 percent and not more than 120.0 percent of
the labeled amount of C11H12Cl2N2O5.
Packaging and storage—Preserve in tight containers.
Labeling—Label Tablets to indicate that they are for veteri-
nary use only and are not to be used in animals raised for
food production.
USP Reference standards 〈11〉—
USP Chloramphenicol RS
Identification—The retention time of the major peak in
the chromatogram of the Assay preparation corresponds to
that in the chromatogram of the Standard preparation as
obtained in the Assay.
Disintegration 〈701〉: 60 minutes.
Uniformity of dosage units 〈905〉: meet the require-
ments.
Official from August 1, 2018
Copyright (c) 2018 The United States Pharmacopeial Convention. All rights reserved.
USP 41
Assay—
Mobile phase and Chromatographic system—Proceed as di-
rected in the Assay under Chloramphenicol.
Standard preparation—Transfer about 25 mg of USP
Chloramphenicol RS, accurately weighed, to a 200-mL volu-
metric flask, add 10 mL of water, and heat on a steam bath
until completely dissolved. Cool to room temperature, dilute
with Mobile phase to volume, and mix. Filter a portion of
this solution through a 0.5-µm or finer porosity filter, and
use the clear filtrate as the Standard preparation.
Assay preparation—Weigh and finely powder not less
than 20 Tablets. Transfer an accurately weighed portion of
the powder, equivalent to about 500 mg of chlorampheni-
col, to a 200-mL volumetric flask, add 80 mL of water, and
heat on a steam bath for 20 minutes, with occasional mix-
ing. Cool to room temperature, dilute with water to vol-
ume, and mix. Transfer 5.0 mL of the resulting solution to a
100-mL volumetric flask, dilute with Mobile phase to vol-
ume, and mix. Filter a portion of this solution through a
0.5-µm or finer porosity filter, and use the clear filtrate as
the Assay preparation.
Procedure—Proceed as directed for Procedure in the Assay
under Chloramphenicol. Calculate the quantity, in mg, of
C11H12Cl2N2O5 in the portion of Tablets taken by the
formula:
4C(rU / rS)
in which the terms are as defined therein.
Chloramphenicol and Hydrocortisone
.
Acetate for Ophthalmic Suspension
» Chloramphenicol and Hydrocortisone Acetate
for Ophthalmic Suspension is a sterile, dry mix-
ture of Chloramphenicol and Hydrocortisone
Acetate with or without one or more suitable
buffers, diluents, and preservatives. It contains
not less than 90.0 percent and not more than
130.0 percent of the labeled amount of chloram-
phenicol (C11H12Cl2N2O5), and not less than
90.0 percent and not more than 115.0 percent of
the labeled amount of hydrocortisone acetate
(C23H32O6), when constituted as directed.
Labeling—If packaged in combination with a container of
solvent, label it with a warning that it is not for injection.
USP Reference standards 〈11〉—
USP Chloramphenicol RS
USP Hydrocortisone Acetate RS
Identification—The retention times of the major peaks in
the chromatogram of the Assay preparation correspond to
that in the chromatogram of the Standard preparation as
obtained in the Assay.
Sterility Tests 〈71〉—It meets the requirements when
tested as directed for Membrane Filtration under Test for Ste-
rility of the Product to be Examined.
pH 〈791〉: between 7.1 and 7.5, in an aqueous suspen-
sion containing 5 mg of chloramphenicol per mL.
Assay—
Mobile phase and Chromatographic system—Proceed as di-
rected in the Assay under Chloramphenicol.
Standard preparation—Transfer about 37.5 mg of USP
Chloramphenicol RS and 37.5J mg of USP Hydrocortisone
Acetate RS, both accurately weighed, J being the ratio of
the labeled amount, in mg, of hydrocortisone acetate to the
Accessed from 36.71.237.98 by belmont7 on Mon Nov 26 09:25:31 EST 2018
USP 41
labeled amount, in mg, of chloramphenicol in the Chloram-
phenicol and Hydrocortisone Acetate for Ophthalmic Solu-
tion, to a 100-mL volumetric flask, add 15 mL of water and
75 mL of methanol, sonicate for a few seconds, dilute with
methanol to volume, and mix. Transfer 5.0 mL of the result-
ing solution to a 25-mL volumetric flask, dilute with Mobile
phase to volume, and mix. Filter a portion of this solution
through a 0.5-µm or finer porosity filter, and use the clear
filtrate as the Standard preparation.
Assay preparation—Transfer the contents of an accurately
counted number of containers of Chloramphenicol and Hy-
drocortisone Acetate for Ophthalmic Solution, equivalent to
about 37.5 mg of chloramphenicol, to a 100-mL volumetric
flask with the aid of 5 mL of water for each 12.5 mg of
chloramphenicol contained therein. Wash each container
with methanol, and add the washings to the volumetric
flask. Dilute with methanol to volume, and mix. Transfer
5.0 mL of the resulting solution to a 25-mL volumetric flask,
dilute with Mobile phase to volume, and mix. Filter a portion
of this solution through a 0.5-µm or finer porosity filter, and
use the clear filtrate as the Assay preparation.
Procedure—Proceed as directed for Procedure in the Assay
under Chloramphenicol. Calculate the quantity, in mg, of
chloramphenicol (C11H12Cl2N2O5) in each container taken by
the formula:
0.5(C / N)(rU / rS)
in which N is the number of containers taken, and the other
terms are as defined therein. Calculate the quantity, in mg,
of hydrocortisone acetate (C23H32O6) in each container taken
by the formula:
500(C / N)(rU / rS)
in which C is the concentration, in mg per mL, of USP Hy-
drocortisone Acetate RS in the Standard preparation, N is the
number of containers taken, and rU and rS are the hydrocor-
tisone acetate peak responses obtained from the Assay prep-
aration and the Standard preparation, respectively.
.
Chloramphenicol and Polymyxin B
Sulfate Ophthalmic Ointment
DEFINITION
Chloramphenicol and Polymyxin B Sulfate Ophthalmic Oint-
ment contains NLT 90.0% and NMT 120.0% of the la-
beled amount of chloramphenicol (C11H12Cl2N2O5) and
NLT 90.0% and NMT 125.0% of the labeled amount of
polymyxin B.
IDENTIFICATION
• A. The retention time of the major peak of the Sample
solution corresponds to that of the Standard solution, as
obtained in the Assay.
ASSAY
• CHLORAMPHENICOL
Mobile phase: Methanol, glacial acetic acid, and water
(450:1:550)
Standard stock solution: 0.25 mg/mL of USP Chloram-
phenicol RS in methanol
Standard solution: 0.1 mg/mL of USP Chloramphenicol
RS from the Standard stock solution in Mobile phase.
Pass through a suitable filter, and use the clear filtrate.
Sample stock solution: Nominally 0.25 mg/mL of
chloramphenicol prepared as follows. Transfer a portion
Official from August 1, 2018
Copyright (c) 2018 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Chloramphenicol 867
of Ophthalmic Ointment containing nominally 25 mg
of chloramphenicol to a suitable conical flask. Add
20 mL of cyclohexane, mix, and sonicate for 2 min.
Add 60 mL of methanol. Filter this mixture, collecting
the filtrate in a 100-mL volumetric flask. Wash the filter
with methanol, collecting the washings in the volumet-
ric flask. Dilute with methanol to volume. Transfer
50.0 mL of the resulting solution to a suitable round-
bottom flask, and evaporate to dryness by rotating the
flask under vacuum in a water bath at 35°. Dissolve the
residue in 50.0 mL of methanol.
Sample solution: Nominally 0.1 mg/mL of chloram-
phenicol from the Sample stock solution in Mobile phase.
Pass through a suitable filter, and use the clear filtrate.
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: LC
Detector: UV 280 nm
Column: 4.6-mm × 10-cm; 5-µm packing L1
Flow rate: 1 mL/min
Injection volume: 10 µL
System suitability
Sample: Standard solution
Suitability requirements
Tailing factor: NMT 2.0
Relative standard deviation: NMT 1.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of
chloramphenicol (C11H12Cl2N2O5) in the portion of
Ophthalmic Ointment taken:
Result = (rU/rS) × (CS/CU) × P × F × 100
rU = peak height from the Sample solution
rS = peak height from the Standard solution
CS = concentration of USP Chloramphenicol RS in
the Standard solution (mg/mL)
USP Monographs
CU = nominal concentration of chloramphenicol in
the Sample solution (mg/mL)
P = potency of chloramphenicol in USP
Chloramphenicol RS (µg/mg)
F = conversion factor, 0.001 mg/µg
Acceptance criteria: 90.0%–120.0%
• POLYMYXIN B
(See Antibiotics—Microbial Assays 〈81〉.)
Sample solution: Shake a portion of Ophthalmic Oint-
ment containing nominally 5000 Polymyxin B Units
with 50 mL of ether in a separator. Extract with four
20-mL portions of Buffer B.6. Combine the aqueous ex-
tracts in a 100-mL volumetric flask, and dilute with
Buffer B.6 to volume.
Analysis: Proceed as directed in the chapter. Dilute the
Sample solution with Buffer B.6 to obtain a Test Dilution
having a concentration that is nominally equivalent to
the median level of the standard.
Acceptance criteria: 90.0%–125.0%
SPECIFIC TESTS
• STERILITY TESTS 〈71〉: Meets the requirements
• OTHER REQUIREMENTS: It meets the requirements for Par-
ticulate and Foreign Matter in Ophthalmic Products—Qual-
ity Tests 〈771〉, Drug Product Quality, Universal Tests, Par-
ticulate and Foreign Matter.
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in collapsible
ophthalmic ointment tubes.