Printed on: Sun Jul 25 2021, 05:14:40 PM Official Status: Currently Official on 25-Jul-2021 DocId: 1_GUID-8E49E2C9-2279-44C6-B23B-3A457D3C7C0E_4_en-US
(EST)
Printed by: Le Tran Official Date: Official as of 01-May-2020 Document Type: USP @2021 USPC
1
Residue on ignition á281ñ: not more than 0.2%.
Methyclothiazide Chloride á221ñ—Shake 750 mg with 25 mL of water for 2
minutes, filter through a suitable membrane filter, and add
4 or 5 drops of 2 N nitric acid: the acidified filtrate shows no
more chloride than corresponds to 0.20 mL of 0.020 N
hydrochloric acid (0.02%).
Selenium á291ñ: 0.003%.
Diazotizable substances—
Standard preparation—Transfer about 10 mg of USP
Methyclothiazide Related Compound A RS, accurately
weighed, to a 50-mL volumetric flask, dilute with acetonitrile
to volume, and mix. Pipet 25 mL of the solution into a 100-mL
C9H11Cl2N3O4S2 360.24 volumetric flask, dilute with acetonitrile to volume, and mix.
Each mL of Standard preparation contains about 50 µg of the
2H-1,2,4-Benzothiadiazine-7-sulfonamide, 6-chloro-3-
Reference Standard.
(chloromethyl)-3,4-dihydro-2-methyl-, 1,1-dioxide, (±)-.
Test preparation—Transfer about 500 mg of
(±)-6-Chloro-3-(chloromethyl)-3,4-dihydro-2-methyl-2H-
Methyclothiazide, accurately weighed, to a 100-mL
1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide [135-
volumetric flask, dissolve in and dilute with acetonitrile to
07-9].
volume, and mix.
Procedure—Pipet 2 mL each of the Standard preparation and
» Methyclothiazide contains not less than 97.0 the Test preparation into separate 50-mL volumetric flasks.
percent and not more than 102.0 percent Pipet 2 mL of acetonitrile into a third 50-mL flask to provide
al
of C9H11Cl2N3O4S2, calculated on the dried basis. the blank. To each flask add 4 mL of 0.1 N hydrochloric acid,
and mix. Add 3.0 mL of sodium nitrite solution (1 in 200) to
Packaging and storage—Preserve in well-closed each flask, mix, and place the flasks in an ice bath for 5
containers. minutes, shaking occasionally. Add to each flask 3.0 mL of
USP Reference standards á11ñ—
ci ammonium sulfamate solution (1 in 50), mix, and allow the
USP Methyclothiazide RS flasks to remain in the ice bath for 1 additional minute. Remove
USP Methyclothiazide Related Compound A RS the flasks from the ice bath, add 1.0 mL of N-(1-naphthyl)
4-Amino-6-chloro-N3-methyl-m-benzenedisulfonamide. ethylenediamine dihydrochloride solution (1 in 1000), and
C7H10ClN3O4S2 299.76 mix. Allow the flasks to stand at room temperature for 1
minute, then dilute with water to volume, and mix.
Identification—
ffi
Concomitantly determine the absorbances of the solutions
obtained from the Standard preparation and the Test
Change to read: preparation in 1-cm cells at 525 nm, with a suitable
A: ▲Spectroscopic Identification Tests á197ñ, Infrared spectrophotometer, using the reagent blank to set the
Spectroscopy: 197K▲ (CN 1-May-2020). instrument. The absorbance of the solution from the Test
preparation does not exceed that of the solution from the
O
Change to read:
Standard preparation, corresponding to not more than 1.0%
of diazotizable substances.
B: ▲Spectroscopic Identification Tests á197ñ, Assay—Transfer about 350 mg of Methyclothiazide,
Ultraviolet-Visible Spectroscopy: 197U▲ (CN 1-May-2020)— accurately weighed, to a 250-mL conical flask, add 40 mL of a
Solution: 20 µg per mL. 1 in 20 solution of potassium hydroxide in methanol, and
Medium: methanol. reflux at full boil for 1 hour. Cool, rinse the inner walls of the
C: Fuse about 100 mg of it with a pellet of sodium condenser with 20 mL of water and two 20-mL portions of
hydroxide: the ammonia fumes produced turn moistened red methanol, add 10 mL of glacial acetic acid and 2 drops of
litmus paper blue. The fused mixture responds to the test for eosin Y TS, and titrate with 0.1 N silver nitrate VS to the first
Sulfite á191ñ. appearance of a definite pink color. Each mL of 0.1 N silver
Loss on drying á731ñ—Dry it at 105° for 4 hours: it loses not nitrate is equivalent to 36.02 mg of C9H11Cl2N3O4S2.
more than 0.5% of its weight.
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