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b Ethyl 2-(6-amino-2,3-dichlorobenzylamino)acetate.
(See Chromatography 〈621〉, System Suitability.)
.
d Ethyl 2-(5,6-dichloro-2-imino-1,2-dihydroquinazolin-3(4H)-yl)acetate
Detector: UV 254 nm
.
hydrobromide.
Column: 4.6-mm × 15-cm; 4-µm packing L11 e 6,7,8-Trichloro-3,5-dihydroimidazo[2,1-b]quinazolin-2(1H)-one.
Autosampler temperature: 5°
.
Anagrelide related
compound Ab 0.55 0.37 0.15 prepared from the contents of NLT 20 Capsules. Add
Diluent (80% of the volume of the flask), sonicate for
.
d Ethyl 2-(5,6-dichloro-2-imino-1,2-dihydroquinazolin-3(4H)-yl)acetate
.
hydrobromide.
e 6,7,8-Trichloro-3,5-dihydroimidazo[2,1-b]quinazolin-2(1H)-one.
.
USP Monographs
Anagrelide Hydrochloride RS, equivalent to 25.00 mg of 80% of the volume of the flask, sonicate for 10 min,
anagrelide, to a 100-mL volumetric flask. Add about stir for about 15 min, and dilute with Diluent to vol-
80 mL of acetonitrile and 3 drops of 2 N hydrochloric ume. Centrifuge (about 4000 rpm) the solution for 15
acid. Sonicate until dissolved. Dilute with acetonitrile to min, and use the supernatant for analysis.
volume. Dilute this solution with Medium to obtain a Chromatographic system
final concentration of about (L/1000) mg/mL, where L (See Chromatography 〈621〉, System Suitability.)
is the Capsule label claim in mg. Mode: LC
Sample solution: Pass a portion of the solution under Detector: UV 254 nm
test through a suitable filter of 0.45-µm pore size. Column: 4.6-mm × 15-cm; 4-µm packing L11
Chromatographic system Column temperature: 45°
(See Chromatography 〈621〉, System Suitability.) Flow rate: 1.0 mL/min
Mode: LC Injection size: 30 µL
Detector: UV 274 nm System suitability
Column: 4.6-mm × 15-cm; 5-µm packing L7 Samples: System suitability solution and Standard
Sample cooler temperature: 5° solution
Flow rate: 1.0 mL/min Suitability requirements
Injection size: 20 µL Resolution: NLT 2.0 between anagrelide hydrochlo-
System suitability ride and anagrelide related compound C, and be-
Sample: Standard solution tween anagrelide hydrochloride and anagrelide re-
Suitability requirements lated compound A, System suitability solution
Column efficiency: NLT 3000 theoretical plates Column efficiency: NLT 3000 theoretical plates,
Tailing factor: NMT 2.0 Standard solution
Relative standard deviation: NMT 2.0% Tailing factor: NMT 2.0, Standard solution
Calculate the percentage of anagrelide dissolved: Relative standard deviation: NMT 2.0% for the
anagrelide peak, Standard solution
Result = (rU/rS) × WS(100 – WC)/(25 × 100) × Mr1/Mr2 × Calculate the percentage of each impurity in the por-
V/L x 100 tion of Capsules taken:
rU = peak response from the Sample solution Result = (rU/rS) × (CS/CU) × (1/F) × 100
rS = peak response from the Standard solution
WS = weight of the USP Anagrelide Hydrochloride rU = peak response of each individual impurity
RS taken (mg) from the Sample solution
WC = water content of the USP Anagrelide rS = peak response of anagrelide from the
Hydrochloride RS (%) Standard solution
Mr1 = molecular weight of anagrelide, 256.10 CU = nominal concentration of anagrelide in the
Mr2 = molecular weight of anagrelide hydrochloride, Sample solution (mg/mL)
292.56
b 6,7,8-Trichloro-3,5-dihydroimidazo[2,1-b]quinazolin-2(1H)-one.
as follows. Transfer 25 mg of Anastrozole to a 50-mL
.
DEFINITION IMPURITIES
Anastrozole contains NLT 98.0% and NMT 102.0% of anas- • RESIDUE ON IGNITION 〈281〉: NMT 0.1%
trozole (C17H19N5), calculated on the anhydrous and sol-
vent-free basis. Delete the following:
IDENTIFICATION •• HEAVY METALS, Method II 〈231〉: NMT 10 ppm• (Official 1-
• A. INFRARED ABSORPTION 〈197K〉 .