Quality Control

ASSIGNMENT NO:1
MONOGRAPHS OF DRUGS ACCORDING TO USP & BP
NAME: Ahmed Raza Khan

ROLL NO: 70116486
SEMESTER: 7-B
SUBJECT: Quality Control
SUBMITTED TO: Ma'am Maryam Shabbir
FACULTY OF PHARMACY
UNIVERSITY OF LAHORE
DRUGS MONOGRAPHS FROM UNITED STATE PHARMACOPEIA
DRUGS FOR OTIC PREPARATION
1. ANTAZOLINE
CHEMICAL STRUCTURE:
STRUCTURAL FORMULA: C17H19N3· H3PO4

SYNONYMS: Antazoline Hydrochloride
CLASSIFICATION: Antazoline is a 1st generation antihistamine with anticholinergic activity.
SPECIFIC TESTS
 PH (791)
Sample: 20 mg/mL
Acceptance criteria: 4.0–5.0
 LOSS ON DRYING (731)
Analysis: Dry at 105° for 4 h.
Acceptance criteria: NMT 0.5%
ASSAY:
Procedure:
Solution A: Dilute 1.0 mL of formic acid with water to 1000 mL.
Mobile phase: Acetonitrile and Solution A (17:83)
Diluent: Acetonitrile and water (17:83)
Standard solution: 0.2 mg/mL of USP Antazoline Phosphate RS in Diluent
System suitability solution: 1 μg/mL of USP Antazoline Related Compound A RS in the
Standard solution
Sample solution: 0.2 mg/mL of Antazoline Phosphate in Diluent Chromatographic system (See
Chromatography (621), System Suitability.)
Mode: LC
Detector: UV 240 nm
Column: 2.1-mm × 10-cm; 1.7-μm packing L11
Temperatures:
Column: 35°
Autosampler: 4°
Flow rate: 0.5 mL/min
Injection volume: 5 μL
System suitability:
Samples: Standard solution and System suitability solution
[NOTE—The relative retention times of antazoline and antazoline related compound A are 1.0
and 1.1, respectively.]
Suitability requirements:
Resolution: NLT 2.0 between antazoline and antazoline related compound A, System suitability
solution
Tailing factor: NMT 1.5 for antazoline, Standard solution
Relative standard deviation: NMT 0.73% for antazoline, Standard solution
Analysis:
Samples: Standard solution and Sample solution
2. AZELASTINE
CHEMICAL STRUCTURE:
STRUCTURAL FORMULA: C22H24ClN3O · HCl

SYNONYMS: Azelastine Hydrochloride
CLASSIFICATION:
TESTS:
 LOSS ON DRYING (731)
Analysis: Dry at 105° to constant weight.
Acceptance criteria: NMT 1.0%
 ACIDITY OR ALKALINITY
Sample solution: 10 mg/mL of Azelastine Hydrochloride in water
Analysis: Add 0.2 mL of bromothymol blue TS to 10 mL of the Sample solution.
Acceptance criteria: NMT 0.1 mL of 0.01 M hydrochloric acid or 0.01 M sodium hydrochloride is
required to produce a color change.
ASSAY:
Produce:
Sample: 300 mg
Blank: 5 mL of anhydrous formic acid and 30 mL of acetic anhydride Titrimetric system (See Titrimetry
(541).)
Mode: Direct titration
Titrant: 0.1 N perchloric acid VS Endpoint detection: Potentiometric
Analysis: In order to avoid overheating in the reaction medium, mix thoroughly throughout and stop the
titration immediately after the endpoint has been reached.
Dissolve the Sample in 5 mL of anhydrous formic acid and add 30 mL of acetic anhydride. Titrate with
Titrant.
Calculate the percentage of azelastine hydrochloride (C 22H24ClN3O · HCl) in the portion of Azelastine
Hydrochloride taken:
Result = {[(VS − VB) × N × F]/W} × 100
VS = Titrant volume consumed by the Sample (mL)
VB = Titrant volume consumed by the Blank (mL)
N = actual normality of the Titrant (mEq/mL)
F = equivalency factor, 41.84 mg/mEq
W = weight of the Sample (mg)
Acceptance criteria: 99.0%–101.0% on the dried basis
DRUGS MONOGRAPHS ACCORDING TO BRITISH PHARMACOPEIA

“DRUGS ACTING ON SKIN”
1. RIFAMPICIN:
CHEMICAL STRUCTURE:
STRUCTURAL FORMULA: C43H58N4O12.

SYNOMYMS:
CLASSIFICATION: Rifampcin antituberculosis drug.
TESTS:
pH (2.2.3)
4.5 to 6.5 for a 10 g/L suspension in carbon dioxide-free water R.
Related substances:
Liquid chromatography (2.2.29). Prepare the test solution and the reference solution immediately before
use.
Solvent mixture To 10 volumes of a 210.1 g\L solution of citric acid monohydrate R add 23 volumes of a
136.1 g\L solution of potassium dihydrogen phosphate R, 77 volumes of a 174.2 g\L solution of
dipotassium hydrogen phosphate R, 250 volumes of acetonitrile R and 640 volumes of water R.
Test solution Dissolve 20.0 mg of the substance to be examined in acetonitrile R and dilute to 10.0 mL
with the same solvent. Dilute 5.0 mL of this solution to 50.0 mL with the solvent mixture.
Reference solution Dissolve 20.0 mg of rifampicin quinone CRS (impurity A) in acetonitrile R and dilute
to 100.0 mL with the same solvent. To 1.0 mL of this solution add 1.0 mL of the test solution and dilute
to 100.0mL with the solvent mixture.
Column:
 size: 1= 0.12 m, -0 =4.6 mm;
 stationary phase: octylsilyl silica gel for chromatography R (5 urn),
 Mobile phase: Mix 35 volumes of acetonitrile Rand 65 volumes of a solution containing 0.1 per
cent V/Vof phosphoric add R, 1;9 g\L of sodium perchlorate R, 5.9 g\L of citric acid
monohydrate R and 20.9 g\L of potassium dihydrogen phosphate R.
 Flow rate 1.5 mL\min.
 Detection Spectrophotometer at 254 nm.
 Injection 20~.
 Run time Twice the retention time of rifampicin.
 System suitabtlity Reference solution: resolution: minimum 4.0 between the peaks due to
rifampicin and impurity A; if necessary, adjust the concentration of acetonitrile in the mobile
phase.
Limits:
 impurity A: not more than 1.5 times the area of the corresponding peak in the chromatogram
obtained with the reference solution (1.5 per cent);
 any other impurity: for each impurity, not more than the area of the peak due to rifampicin in the
chromatogram obtained with the reference solution (1.0 per cent);
 sum of impurities other than A: not more than 3.5 times the area of the peak due to rifampicin in
the chromatogram obtained with the reference solution (3.5 per cent);
 disregard limit: 0.05 times the area of the peak due to rifampicin in the chromatogram obtained
with the reference solution (0.05 per cent).
Loss on drying (2.2.32) Maximum 1.0 per cent, determined on 1.000 g by drying at 80°C at a pressure
not exceeding 0.67 kPa for 4 h.
Sulfated ash (2.4.14) Maximum 0.1 per cent, determined on 2.0 g.

ASSAY:
Dissolve 0.100 g in methanol R and dilute to 100.0 mL with the same solvent. Dilute 2.0 mL of this
solution to 100.0 mL with phosphate buffer solution pH 7.4 R. Measure the absorbance (2.2.25) at the
absorption maximum at 475 nm, using phosphate buffer solution pH 7.4 R as the compensation liquid.
Calculate the content of C43H58 01Z, taking the specific absorbance to be 187.
2. RETINOL:
CHEMICAL SRTUCTURE:
STRUCTURAL FORMULA: C20H30O

SYNONYMS: Isotretinoin
CLASSIFICATION:
TESTS:
Acid value (2.5.1): Maximum 2.0, determined on 2.0 g.
Peroxide value (2.5.5, Method A): Maximum 10.0.
Related substances: The thresholds indicated under Related substances (Table 2034.-1) in the general
monograph Substances for pharmaceutical use (2034) do not apply.
ASSAYS:
Carry out the assay as rapidly as possible, avoiding exposure to actinic light, air, oxidisingagfl1'lts,
oxidation catalysts (e.g. copper, iron), acids and prolonged heat; use freshly prepared solutions. If partial
crystallization has occurred, homogenize the material at a temperature of about 65°C," but avoid
prolonged heating. Carry out the assay according to Method A.
Method A
Ultraviolet absorption spectrophotometry (2.2.25). Dissolve 25-100 mg, weighed with an accuracy of 0.1
per cent, in 5 mL of pentane R and dilute with 2-propanol Rl to a presumed concentration of 10-15
IU/mL. Verify that the absorption maximum of the solution lies between 325 nm and 327 nm and
measure the absorbances at 300 nm, 326 nm, 350 nm and 370 nm. Repeat the readings at each wavelength
and take the mean values. Calculate the ratio AJA326 for each wavelength. If the ratios do not exceed:
0.60 at 300 nm, 0.54 at 350 nm, 0.14 at 370 nm, calculate the content of vitamin A in International Units
per gram using the following expression:
A326 x V x \1900 100 x m
A326 absorbance at 326 nm,
m mass of the preparation to be examined, in grams,
V total volume to which the preparation to be examined is diluted to give 10-15 IU/mL,
1900 factor to convert the specific absorbance of esters of retinol into International Units per gram.

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ASSIGNMENT NO:1

MONOGRAPHS OF DRUGS ACCORDING TO USP & BP

NAME: Ahmed Raza Khan

STRUCTURAL FORMULA: C17H19N3· H3PO4

STRUCTURAL FORMULA: C22H24ClN3O · HCl

DRUGS MONOGRAPHS ACCORDING TO BRITISH PHARMACOPEIA

STRUCTURAL FORMULA: C43H58N4O12.

Sulfated ash (2.4.14) Maximum 0.1 per cent, determined on 2.0 g.

STRUCTURAL FORMULA: C20H30O

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