The document discusses dexamethasone, a synthetic corticosteroid, detailing its properties, manufacturing processes, testing methods, and regulatory compliance for tablet and ophthalmic suspension forms. It describes procedures for content uniformity, dissolution testing, and chromatographic assays to ensure that products contain the appropriate amount of dexamethasone and meet quality standards. It also lists specifications for packaging, storage, and testing results confirming that products comply with the required ranges for efficacy and safety.

1. Pharmaceutical
Quality
Management
Dr. Asra Hameed
Pharm.D (JUW)
asra_hameed1@hotmail.com

3. BP

4. 
Dexamethasone
is a synthetic
(man-made)
corticosteroid.
Corticosteroids
are naturally-
occurring
chemicals
produced by the
adrenal glands
located above
the kidneys.
Corticosteroids
affect the
function of
many cells
within the body
and suppress
the immune
system.
Corticosteroids
also block
inflammation
and are used in
a wide variety
of inflammatory
diseases
affecting many
organs.
The FDA
approved
dexamethasone
in October
1958.
DEXAMETHASONE

5. 
Dexamethasone Tablets Contain Dexamethasone.
CONTENT OF DEXAMETHASONE:
95.0 to 105.0% of the stated amount.
ACTION AND USE:
Glucocorticoid.
DEXAMETHASONE TABLETS

6. 
Powdered
Tablets
containing 20
mg of
dexamethasone
+ 5ml of 0.1M
NaOH.
Add 50ml
dichlorometh
ane mix with
aid of
ultrasound
(20min)
Filter layer of
dichlorometh
ane ,
evaporate it
with using a
rotary
evaporator
Dry residue
at 105℃ for 2
hours.
Check the
absorption at
infrared
spectrum of
the dried
residue.
IDENTIFICATION

7. 
Tablets containing less than 2mg or less
than 2% w/w of dexamethasone
comply with the requirement
Carry out the method for liquid
chromatography
UNIFORMITY OF CONTENT
Tablet +sufficient methanol (50%)
solution of 0.0025% w/v of
dexamethasone
shake (10min)
filter

8. 
(2)
CHROMATOGRAPHICCONDITIONS:
 Stainless steel column
 Isocratic elution
 Flow rate of 1.4ml/min
 Ambient column temperature
 Detection wavelength of 238nm
 Inject 20µL of each solution
0.0025% w/v of dexamethasone
in methanol (50%)

9. 

10. 
Tablets containing less than 2mg or less than 2% w/w
of dexamethasone
ASSAY
Use the average of the 10 individual results
obtained in the test for uniformity of content

11. 
Tablets containing 2mg or more than 2% w/w of
Dexamethasone:
(1)
ASSAY
Powdered tablets + 2.5 mg
dexamethasone + 20ml methanol
shake (20min)
filter

12. 
(2)
STORAGE:
Dexamethasone tablets should be
protected from light
0.0125% w/v of
dexamethasone BPCRS in
methanol 50%

13. USP

14. 
Dexamethasone tablet contains not
less than 90.0 %and not more than
110.0% of the label amount of
dexamethasone.
Packaging And Storage: preserve
in well close container.
Introduction

15. 
Process by
which solvent
enter solid
substance to
yield a solution.
Dissolution
medium:
solvent or
medium in
which
substance is
dissolve.
Medium: dilute
hydrochloric
acid (1
in100ml).
Apparatus
1:100 RPM.
Time:45min.
Standard
solution:
prepare as
directed for std.
preparation and
assay of
steroids, using
dexamethasone
RS.
Dissolution

16. 
Extract a filtered aliquot (dissolution medium) about200 micro
gm. of dexamethasone with 3 portions of
chloroform(15ml).Evaporate this extract to dryness on steam
bath, cool it and dissolve the residue(extract) in 20ml of alcohol.
Calculate the portion in mg of dexamethasone dissolve.
Tolerance: not less than 70% label amount of dexamethasone is
dissolve in 45 minutes.
Procedure

17. 
DIFFERENCE B/W CONTENT
UNIFORMITY & ASSAY
Uniformity of content is by two
methods by weight variation and by
content uniformity.
Weight variation means performing
assay and relating with individual unit
of dosage form.
Content uniformity means for ten
sample (dosage unit) individually
analysed.

18. 
PROCEDURE FOR
CONTENT UNIFORMITY
STANDARD SOLUTION:
Prepare as directed for Standard Preparation under Assay for steroids using USP
Dexamethasone RS.
TEST SOLUTION:
Place 1 tablet in a separator with 15ml of water and swirl to disintegrate
completely.
Extract with four 10ml portion through chloroform-washed cotton into 50ml
volumetric flask.
Add chloroform to volume and mix.
Pipette a volume of this solution equivalent to 200microgram of dexomethasone
into a glass stoppered 50ml conical flask.

19. Proceed as
directed for
Procedure under
Assay for
steroids, except to
allow to stand in
the dark for 45
mins.
Calculate the
quantity in mg of
total steroids as
C22H29FO5 in
the tablet by the
formula:
(C/V)(AU / AS)
In which V is the
volume in ml of
the aliquot taken
to prepare the
Test solution.

20. 
ASSAY
MOBILE SOLVENT:
Prepare a suitable aqueous solution of acetonitrile
approximately 1 in 3 , such that the retention time of
dexomethasone is b/w 3 mins and 6 mins.
STANDARD PREPARATION:
Dissolve an accurately weighd quantity of USP
Dexamethasone RS in dilute methanol to obtain a solution
having a known concentration of about 0.1 mg per ml.

21. ASSAY PREPARATION:
Weigh and finely powder not fewer than 10 tablets.
Weigh accurately a portion of powder equivalent to about 5 mg
of dexamethasone.
Transfer to a 50ml volumetric flask and add 30 ml of dilute
methanol.
Sonicate the flask for about 2 mins , shake by mechanical means for 30 mins.
Dilute with the same solvent to volume.
Filter a portion of mixture through a suitable filter to obtain a clear filtrate.

22. PROCEDURE
Introduce equal volumes of the Assay preparation and the Standard
preparation into a high pressure liquid chromatograph operated at room
temperature by means of a loop injector, adjusting the specimen size other
operating parameters such that the peak obtained with the Standard
preparation is about 0.6 full scale.
The apparatus is fitted with a 4.6 mm × 30 cm column packed with packing L1
and is equipped with an UV detector capable of monitoring absorption at 254
nm and a suitable recorder.
In a suitable chromatogram , the coefficient of variation for five replicate
injections of a single specimen is not more than 3 %.

23. Measure the
responses of the
peaks at
identical
retention times
obtained with
the Assay
preparation and
the Standard
preparation.
Calculate the
quantity in mg
of C22H29FO5
in the portion of
tablets taken
by the formula:
50C(ru/rs)
In which C= is
the
concentration
in mg per ml of
USP
Dexamethasone
RS in the
Standard
preparation .
ru and rs = are
the peak
responses
obtained from
the Assay
preparation
and the
Standard
preparation.

24. BP

25. 
Dexamethasone suspension: a sterile suspension of
dexamethasone in a suitable vehicle.
CONTENT OF DEXAMETHASONE:
95.0 to 105.0% of the stated amount.
ACTION AND USE:
Glucocorticoid.
Introduction:

26. 
Eye drop
containing 20 mg
of dexamethasone
+ 5ml of 0.1M
NaOH.
Add 50ml
dichloromethane
mix with aid of
ultrasound
(20min)
Filter layer of
dichloromethane ,
evaporate it with
using a rotary
evaporator
Dry residue at
105℃ for 2 hours.
Check the
absorption at
infrared spectrum
of the dried
residue.
IDENTIFICATION

27. 
PARTICLE SIZE
Examine using an automated light obscuration instrument
Not more than 20 particle >25µm
Not more than 2 particle >50µm
No particles >90µm.
ACIDITY
pH,5.0 to 6.0
TESTS:

28. 
•Carry out the method for Liquid chromatography
•Dispense a quantity of eye drop containing 20mg of dexamethasone in 70ml of
mobile phase, mix the aid of ultrasound for 10 min, dilute with sufficient water to
produce 100 ml and filter.
•0.02% w/v of dexamethasone BPCRS
•0.01% w/v of dexamethasone impurity standard BPCRS.
ASSAY

29. 
Related susbstance may be used :
SYSTEM STABILITY:
Test in not valid unless chromatogram obtained with solution (3).
Resolution factor between the peaks id due to impurity 3 and
dexamethasone is atleast 1.5
the chromatogram supplied with dexamethasone impurity standard
BPGRS.
CHROMATOGRAPHIC
CONDITIONS:

30. •Calculate the content of
C22H29FO5 in the eyedrop
using the declared content of
C22H29FO5 in
dexamethasone BPGRS.
DETERMINATION
OF CONTENT
•Should be stored in
accordance with
manufacturer’s instructions.
STORAGE

31. 
Dexamethsone-17ß-
carboxylic acid.
Dexamethasone-21-
aldehyde.
Dexamethasone-17αdehydroxy-
17ß-carboxylic acid.
IMPURITIES

32. USP

33. 131027

34. 
Dexamethasone ophthalmic suspension of
dexamethasone containing a suitable
antimicrobial preservative
It may contain suitable buffers, stabilizers and
suspending and viscosity agent
It contains not less than 90.0 percent and not
more than 110.0 percent of the labeled amount
of 22H29FO5
INTRODUCTION

35. 
Preserve in tight
containers
PACKAGING AND
STORAGE

36. 
Transfer a volume of ophthalmic suspension equivalent to about
2.5 mg of dexamethasone to a test tube ,add ml of chloroform and
shake.
Centrifuge and apply 10µL of the chloroform layer and 10µL of a
standard solution of usp .Dexamethasone RS in chloroform
containing 500µg per ml on a thin layer chromatographic plate
coated with a 0.25mm layer of chromatographic silica gel mixture
Develop the chromatogram in solvent A as directed under single
steroid assay
IDENTIFICATION:

37. 
Mark the solvent front
and locate the spots on
the plate by spraying
with a 1 in 5 solution of
p-toluene sulfonic acid
in a mixture of 9
volume of alcohol and
volume of propylene
glycol and heating until
spots appear
The Rf value of
the principal spot
obtained from
the solution
under test
corresponds to
that obtained
from the
standard solution

38. 
STERILITY
Should be meet the requirement
Media Membrane
Filtration
Aqueous
Solutions
Direct
Inoculation of
the Culture
Media
Observation And
Interpretation Of
Results
Rabbit
Pyrogen Test
Pyrogen Test Spark Test Leaker Test

39. The pH should be
between 5.0 and 6.0

40. 
ASSAY
MOBILE PHASE
water
acetonitrile
(60:40)
STANDARD PREPARATION
USP Dexamethasone RS
mobile phase
dilute if necessary
concentration of 0.12 mg/mL

41. ASSAY
ASSAY PREPARATION
measured volume of Opthalmic
Suspension (3mg of
dexamethasone)
25 mL volumetric flask
dilute with mobile phase to
volume & mix
CHROMATOGRAPHIC SYSTEM
254-nm detector
4.6-mm*25-cm column (packing L1)
Flow rate is about 2 mL/min
Chromatograph standard
preparation & record peak response
column efficiency is not
< 1750 , tailing factor is not
> 3.0 & the relative SD for replicate
injection is not > 3.0%

42. Separately inject equal volumes of the standard preparation
and the assay preparation into the chromatograph, record
the chromatographs and measure the responses for the
major peaks.Calculate the quantity in mg of Dexamethasone
in each mL of the opthalmic suspension using formula:
25(C/V)(ru/rs)

44. 
TEST RANGE/ LIMIT RESULT
COMMENTS/
REMARKS
Identification
IR spectrum
Concordant with
RS 089
Concordant. Identified.
Uniformity of
content
L1 (maximum
allowed
acceptance
value) is 15
A.V= 5.6 Accepted.
Assay 95-105% 97% Accepted.
Dexamethasone tablets
BP

45. 
TEST RANGE/ LIMIT RESULT
COMMENTS/
REMARKS
Identification
RF value corresponds
to standard.
Corresponded. Identified.
Dissolution
Not less than 70% of
labeled amount of
C22H29FO5 is
dissolved in
45minutes.
85% C22H29FO5
is dissolved.
Passed.
Uniformity of
dosage units
L1 (maximum
allowed acceptance
value) is 15
A.V = 5.6 Accepted.
Assay 90-110 % 97% Accepted.
Dexamethasone tablets
USP

46. 
DEXAMETHSONE OPTHALMIC
SUSPENSION BP
TEST RANGE/ LIMIT RESULT
COMMENTS/
REMARKS
Identification
IR spectrum Concordant
with RS 089
Concordant. Identified.
Particle size
Not more than 20 particles
>25µm
Not more than 2particles
>50µm
No particle >90µm
19paricles are
>25µm
1 particle is
>50µm
No particle is
>90µm
Accepted.
Acidity pH 5.0-6.0 pH is 5.6 Accepted.
Assay 95-105% 97% Accepted.

47. 
DEXAMETHSONE OPTHALMIC
SUSPENSION USP
TEST RANGE/ LIMIT RESULT
COMMENTS/
REMARKS
Identification
RF value corresponds
to standard.
Corresponded. Identified.
Sterility
Should be no
evidence of microbial
growth.
The product
complies with
the test for
sterility.
Passed the
sterility test.
pH 5.0-6.0 pH is 5.6 Accepted.
Assay 90-110 % 97% Accepted.

48. 

49. The End 