562 Monographs, Part I

Wavelength: 283.3 nm. (0.1 g, methanol, 10 mL, 100 mm)

(5) Arsenic—Prepare the control solution with 1.0
g of Ferrous Sulfate Hydrate according to Method 1,
and perform the test (not more than 2 ppm).
Assay Weigh accurately about 0.7 g of Ferrous Sul-
fate Hydrate, add 20 mL of water, 20 mL of dilute sul-
furic acid TS and 2 mL of phosphoric acid, and imme-
diately titrate with 0.02 mol/L potassium permanganate
VS.
Each mL of 0.02 mol/L potassium permanganate VS
= 27.80 mg of FeSO4·7H2O
Containers and Storage Containers—Tight con-
tainers.
Purity (1) Heavy metals⎯Proceed with 1.0 g of
Finasteride according to Method 2 and perform the test.
Prepare the control solution with 1.0 mL of standard
lead solution (not more than 10 ppm).
(2) Related substances—Dissolve about 0.1 g of
Finasteride, accurately weighed, in a mixture of water
and acetonitrile (1 : 1) to make exactly 100 mL and use
this solution as the test solution. Perform the test with
15 μL of the test solution as directed under Liquid
Chromatography according to the following operating
conditions and determine the area of each peak by the
automatic integration method and calculate the amount
of each related substance: the amount of any related
subtances is not more than 0.5 % and the total amount
of related substances is not more than 1.0 %.

Ai
Amount (%) of each related substance = 100 × A
Finasteride s

CH3 Ai: Peak area of each related substance

H
O
N
CH3 As: Sum of all peak area obtained from the test so-
CH3 lution
CH3
H

CH3 H
H H
O N
H H
C23H36N2O2: 372.54
(1S,3aS,3bS,5aR,9aR,9bS,11aS)-N-tert-Butyl-9a,11a-
dimethyl-7-oxo-1,2,3,3a,3b,4,5,5a,6,9b,10,11-
dodecahydroindeno[5,4-f]quinoline-1-carboxamide
[98319-26-7]
Finasteride contains not less than 98.5 % and not more
than 101.0 % of finasterid (C23H36N2O2), calculated on
the anhydrous basis.
Description Finasteride appear as white or grayish
white crystalline powder.
Finateride is freely soluble in ethanol (95), or in chlo-
roform, and very slightly soluble in water.
Melting point―about 257 ºC
Identification (1) Determine the infrared spectra of
Finateride and Finasteride RS, as directed in the paste
method under Infrared Spectrophotometry: both spec-
tra exhibit similar intensities of absorption at the same
wavenumbers.
(2) The retention time of the principal peak ob-
tained from the test solution under Assay is equal to
that of the principal peak obtained from the standard
solution.
Specific Optical Rotation [α] 25 : -56.0 ~ -60.0°
405nm
Operating conditions
Detector : An ultraviolet absorption photometer
(wavelength: 210 nm).
Column : A stainless steel column, about 4.6 mm in
internal diameter and about 30 cm in length, packed
with octadecylsilanized silica gel for liquid chromatog-
raphy (4 μm in particle diameter).
Mobile phase : A mixture of water, tetrahydrofuran
and acetonitrile (8 : 1 : 1)
Column temperature: A constant temperature of
about 60 °C
Flow rate: 1.5 mL/minute
System suitability
System performance: Dissolve 10 mg of
Finasteride RS in a mixture of water and acetonitrile
(1 : 1) to make 10 mL. When the procedure is run with
15 μL of this solution under the above operating condi-
tions, the number of theoretical plates and symmetry
factor of the peak of finasteride are not less than 10000
and not more than 1.3, respectively.
Water Not more than 0.3 % (1 g, volumetric titration,
direct titration).
Residue on Ignition Not more than 0.1 % (1 g).
Assay Dissolve about 20 mg each of Finateride and
Finasteride RS, accurately weighed, in a mixture of
water and acetonitrile (1 : 1) to make exactly 100 mL
and use these solutions as the test solution and the
standard solution, respectively. Perform the test with
10 μL each of the test solution and the standard solu-
tion as directed under Liquid Chromatography accord-
ing to the following operating conditions and deter-
mine the peak areas, AT and AS, of the principal peak
 KP X 563

for the test solution and the standard solution, respec- Description Flavin Adenine Dinucleotide Sodium is
tively. an orange-yellow to pale yellow-brown powder, is
odorless or has a slight, characteristic odor and has a
Amount (mg) of finasteride (C23H36N2O2) slightly bitter taste.
AT Flavin Adenine Dinucleotide Sodium is freely soluble
= Amount (mg) of Finasteride RS × A in water and practically insoluble in methanol, in etha-
S
nol (95), in ethylene glycol or in ether.
Operating conditions Flavin Adenine Dinucleotide Sodium is hygroscopic.
Detector : An ultraviolet absorption photometer Flavin Adenine Dinucleotide Sodium is decomposed
(wavelength: 215 nm). by light.
Column : A stainless steel column, about 3.0 mm in
internal diameter and about 30 cm in length, packed Identification (1) A solution of Flavin Adenine Di-
with octylsilanized silica gel for liquid chromatography nucleotide Sodium (1 in 100000) is pale yellow-green
(3 μm in particle diameter). in color and shows a strong yellow-green fluorescence.
Mobile phase : A mixture of water and Take 5 mL of the solution, and add 20 mg of hydrosul-
tetrahydrofuran (4 : 1) fite sodium: the color and the fluorescence of the solu-
Flow rate: about 3 mL/minute tion disappear and gradually reappear when the solu-
System suitability tion is shaken in air. Add dilute hydrochloric acid or
System performance: When the procedure is run sodium hydroxide TS drop-wise: the fluorescence of
with 10 μL of the standard solution under the above the solution disappears.
operating conditions, the number of theoretical plates (2) Determine the infrared spectrum of Flavin Ade-
and symmetry factor of the peak of finasteride are not nine Dinucleotide Sodium and Flavin Adenine Dinu-
less than 1800 and not more than 1.3, respectively. cleotide Sodium RS as directed in the potassium bro-
System reproducibility: When the test is repeated mide disk method under Infrared Spectrophotometry:
5 times with 10 μL each of the standard solution under both spectra exhibit similar intensities of absorption at
the above operating conditions, the relative deviation the same wavenumbers.
of the peak area is not more than 1.0 %. (3) Take 0.1 g of Flavin Adenine Dinucleotide So-
dium, add 10 mL of nitric acid, evaporate on a water-
Containers and Storage Containers—Tight con- bath to dryness and ignite. To the residue, add 10 mL
tainers. of diluted nitric acid (1 in 50), boil for 5 minutes and
after cooling, neutralize with ammonia TS, then filter
the solution, if necessary: the solution responds to the
Qualitative Tests for sodium salt and the Qualitative
Flavin Adenine Dinucleotide Tests (1) and (3) for phosphate.
Sodium Specific Optical Rotation [α ] 20D : -21.0 ~ -25.5° (0.3
NH2 g, calculated on the anhydrous basis, water, 20 mL, 100
N mm).
N

N N pH Dissolve 1.0 g of Flavin Adenine Dinucleotide

H H H ONa ONa
Sodium in 100 mL of water: the pH of this solution is
H2C C C C CH2O P O P OCH2 between 5.5 and 6.5
OH OH OH O O
O
H3C N N O Purity (1) Clarity and color of solution—Dissolve
H
H H
H
0.20 g of Flavin Adenine Dinucleotide Sodium in 10
H3C N
NH
OH OH mL of water: the solution is clear and orange-yellow in
O
color.
(2) Free phosphoric acid—Weigh accurately about
C27H31N9Na2O15P2: 829.51 20 mg of Flavin Adenine Dinucleotide Sodium, dis-
solve in 10 mL of water and use this solution as the test
Disodium adenosine 5'-(3-{D-ribo-5-[7,8-dimethyl- solution. Separately, measure exactly 2 mL of standard
2,4-dioxo-3,4-dihydrobenzo[g]pteridin-10(2H)-yl]- phosphoric acid solution, add 10 mL of water and use
2,3,4-trihydroxypentyl} dihydrogen diphosphate) this solution as the standard solution. To each of the
[84366-81-4] test solution and the standard solution, add 2 mL of
diluted perchloric acid (100 in 117), then add 1 mL of
Flavin Adenine Dinucleotide Sodium contains not less ammonium molybdate TS and 2 ml of 2,4-
than 93.0 % and not more than 101.0 % of flavin ade- diaminophenol hydrochloride TS, respectively, shake,
nine dinucleotide sodium (C27H31N9Na2O15P2), calcu- add water to make exactly 25 mL and allow to stand at
lated on the anhydrous basis. 20 ± 1 ºC for 30 minutes. Perform the test with the test
solution and the standard solution as directed under