Printed on: Tue Aug 03 2021, 07:37:30 AM Official Status: No Longer Official on 03-Aug-2021
(EST)
Printed by: Le Tran Official Date: Omitted on 01-May-2021
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Zalcitabine Tablets
» Zalcitabine Tablets contain not less than 90.0
percent and not more than 110.0 percent of the
labeled amount of zalcitabine (C9H13N3O3).
[CAUTION—Great care should be taken to prevent
inhaling particles of zalcitabine and exposing it to
the skin.]
Packaging and storage—Preserve in tight, light-resistant
containers.
USP Reference standards á11ñ—
USP Zalcitabine RS
USP Zalcitabine Related Compound A RS
2′,3′-Didehydro-2′,3′-dideoxycytidine.
Identification—The retention time of the major peak in the
chromatogram of the Assay preparation corresponds to that of
the Standard preparation, as obtained in the Assay.
Dissolution á711ñ—
Medium: water; 900 mL.
Apparatus 2: 50 rpm.
Time: 20 minutes.
Phosphate buffer—Transfer 8.7 g of dibasic potassium
phosphate to a 1 L volumetric flask, dilute with water to
er
volume, and adjust with phosphoric acid to a pH of 6.8.
Mobile phase—Prepare a filtered and degassed mixture of
Phosphate buffer, methanol, and acetonitrile (96:4:3). Make
adjustments if necessary (see System Suitability under
Chromatography á621ñ).
Standard preparation—Transfer about 10 mg of USP
ng
Zalcitabine RS, accurately weighed, to a 250-mL volumetric
flask. Add about 200 mL of Medium, and sonicate until
complete solution is effected. Dilute with Medium to volume,
and mix.
Chromatographic system (see Chromatography á621ñ)—
The liquid chromatograph is equipped with a 270-nm
detector and a 3.9-mm × 15-cm column that contains 10-µm
packing L1. The flow rate is about 1 mL per minute.
Lo
Chromatograph the Standard preparation, and record the
peak responses as described for Procedure: the retention time
is about 5 minutes; the tailing factor is not more than 2; and
the relative standard deviation is not more than 2%.
Procedure—Separately inject equal volumes (about 150 µL)
of the Standard preparation and a filtered portion of the
solution under test into the chromatograph, record the
chromatograms, and measure the responses of the major
peaks. Calculate the quantity, in mg, of zalcitabine in the
Tablets taken by the formula:
o
900C(rU/rS)
in which C is the concentration, in mg per mL, of USP
N
Zalcitabine RS in the Standard preparation; and rU and rS are
the zalcitabine peak responses obtained from the solution
under test and the Standard preparation, respectively.
https://online.uspnf.com/uspnf/document/1_GUID-D4E31763-25A0-41BA-B68C-0D8B5F0F9889_3_en-US
DocId: 1_GUID-D4E31763-25A0-41BA-B68C-0D8B5F0F9889_3_en-US
Document Type: USP @2021 USPC
1
Tolerances—Not less than 80% (Q) of the labeled amount
of C9H13N3O3 is dissolved in 20 minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Assay—
Buffer solution—Dissolve 3.4 g of monobasic potassium
al
phosphate in sufficient water to make 1 L. Using a suitable pH
meter, adjust with phosphoric acid to a pH of 2.2. [NOTE—If
too much phosphoric acid is added, yielding a pH below 2.2,
the pH may be adjusted to 2.2 with 0.025 M monobasic
potassium phosphate.] Add 1.08 g of sodium 1-octanesulfonic
ci
acid, and mix.
Mobile phase—Prepare a filtered and degassed mixture of
Buffer solution and acetonitrile (85:15).
Diluent—Prepare a mixture of water and acetonitrile (17:3).
Resolution solution—Dissolve weighed quantities of USP
Zalcitabine RS and USP Zalcitabine Related Compound A RS
ffi
in Diluent, and dilute quantitatively, and stepwise if necessary,
with the same solvent to obtain a solution containing about
0.02 mg per mL of zalcitabine and 0.002 mg per mL of
zalcitabine related compound A.
Standard preparation—Dissolve an accurately weighed
quantity of USP Zalcitabine RS in Diluent, and dilute
O
quantitatively, and stepwise if necessary, with the same solvent
to obtain a solution having a known concentration of about
0.008 mg per mL.
Assay preparation—Transfer 5 Tablets to a volumetric flask
suitable to obtain a solution containing about 0.008 mg
zalcitabine per mL. Add a volume of Diluent that is about
six-tenths of the volume of the flask, sonicate for 15 minutes,
and shake by mechanical means for 10 minutes. Dilute with
Diluent to volume, and mix. Filter before use.
Chromatographic system (see Chromatography á621ñ)—
The liquid chromatograph is equipped with a 280-nm
detector, a precolumn cartridge that contains packing L1,
and a 4.6-mm × 25-cm analytical column that contains 5-µm
packing L1. The flow rate is about 1.5 mL per minute.
Chromatograph the Resolution solution, and record the peak
responses as directed for Procedure: the resolution, R, between
the zalcitabine and zalcitabine related compound A peaks is
not less than 1.1, and the tailing factor for the zalcitabine peak
is not more than 1.5. Chromatograph the Standard
preparation, and record the peak responses as directed for
Procedure: the relative standard deviation for replicate
injections is not more than 2%.
Procedure—Separately inject equal volumes (about 50 µL)
of the Standard preparation and the Assay preparation into the
chromatograph, record the chromatograms, and measure the
responses of the major peaks. Calculate the quantity, in mg,
of C9H13N3O3 in the portion of Tablets taken by the formula:
CV(rU/rS)
in which C is the concentration, in mg per mL, of USP
Zalcitabine RS in the Standard preparation; V is the volume, in
mL, of the volumetric flask used to prepare the Assay
preparation; and rU and rS are the zalcitabine peak responses
obtained from the Assay preparation and the Standard
preparation, respectively.▲ (USP 1-May-2021)
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