NITRAZEPAM IP/BP

C15H11N3O3: 281.27
7-Nitro-5-phenyl-1,3-dihydro-2 H-1,4-benzodiazepin-2-one
[146-22-5 ]

Nitrazepam, when dried,
contains not less than
99.0z of C15H11N3O3.

Melting point: about 227 C (with decomposition).

Description :

Nitrazepam occurs as white to yellow crystals or crystalline powder. It is odorless.It is freely soluble in acetic acid (100), soluble in acetone and in chloroform, slightly soluble in methanol, in ethanol (95) and in ethanol (99.5), very slightly soluble in diethyl ether, and practically insoluble in water.
C) Melting point: about 2279 (with decomposition).

Identification:  (1) To 3 mL of a solution of Nitrazepam in
methanol (1 in 500) add 0.1 mL of sodium hydroxide TS: a
yellow color is produced.

(2) To 0.02 g of Nitrazepam add 15 mL of dilute hydrochloric acid, boil for 5 minutes, cool, and ˆlter: the ˆltrate responds to the Qualitative Tests <1.09> for primary aromatic amines.
(3) Neutralize 0.5 mL of the ˆltrate obtained in (2) with sodium hydroxide TS, add 2 mL of ninhydrin TS, and heat on a water bath: a purple color is produced.
(4) Determine the absorption spectrum of a solution of Nitrazepam in ethanol (99.5)
(1 in 100,000) as directed under Ultraviolet-visible Spectrophotometry <2.24>, and compare the spectrum with the Reference Spectrum: both spectra exhibit similar intensities of absorption at the same wavelengths.

Purity :
(1) Clarity and color of solution—Dissolve 0.10 g of Nitrazepam in 20 mL of acetone: the solution is clear and pale yellow to light yellow in color.
(2) Heavy metals <1.07>—Proceed with 1.0 g of Nitrazepam according to Method 2, and perform the test. Prepare the control solution with 2.0 mL of Standard Lead Solution (not more than 20 ppm).
(3) Arsenic <1.11>—Prepare the test solution with 1.0 g of Nitrazepam according to Method 3, and perform the test (not more than 2 ppm).
(4) Related substances—Dissolve 0.25 g of Nitrazepam in a 10 mL of mixture of methanol and chloroform (1:1), and use this solution as the sample solution. Pipet 1 mL of the sample solution, add a mixture of methanol and chloroform
(1:1) to make exactly 20 mL, pipet 2 mL of this solution, add a mixture of methanol and chloroform (1:1) to make exactly 50 mL, and use this solution as the standard solution. Perform the test with these solutions as directed under Thin-layer Chromatography <2.03>. Spot 10 mL each of the sample solution and standard solution on a plate of silica gel with ‰uorescent indicator for thin-layer chromatography. Develop the plate with a mixture of nitromethane and ethyl acetate
(17:3) to a distance of about 10 cm, and air-dry the plate. Examine under ultraviolet light (main wavelength: 254 nm): the spots other than the principal spot from the sample solution are not more intense than the spot from the standard solution.



Loss on drying <2.41> 4 hours). Residue on ignition <2.44>

Assay Weigh accurately about 0.4 g of Nitrazepam, previously dried, and dissolve in 40 mL of acetic acid (100). Titrate <2.50> with 0.1 mol W perchloric acid VS (potentiometric Ltitration). Perform a blank determination, and make any
necessary correction.

Each mL of 0.1 mol W perchloric acid VS
＝ 28.13 mg of C15H11N3O3

Containers and storage Containers—Tight containers.

Storage—Light-resistant.

Not more than 0.5z (1 g, 1059 C,

Not more than 0.1z (1 g).

Packing: 25kg /drum or on request.

PRODUCT CODE: TAJ API NTWAK 88765323