A Review: Current Analytical Methods for Determination of
Dexamethasone Sodium Phosphate in Pharmaceutical
Dosage Forms and Biological Fluid
Hiral M. Pokiya1*, Priyanka S. Malani1, Bhumi K. Patel1, Dr. Hasumati A. Raj1, Dr. Vinit C. Jain1
1
Shree Dhanvantary Pharmacy College,Kim, Surat, Gujarat
Address For correspondence:
Department of Quality Assurance
Shree Dhanvantary Pharmacy College
At : Kim, Taluka : Olpad, Dist: Surat, Pin code : 394110
Mobile No: 8866109499
*Email: pokiyahiral@yahoo.in
Number of figures: 1
Number of tables: 4
ABSTRACT:
Dexamethasone is a synthetic corticosteroid (glucocorticoid).It has anti-inflammatory action.
Which is available in the different pharmaceutical dosage forms through various routes of
administration, such as oral, topical and systemic. It is used to treat inflammation by relieving
symptoms such as swelling, redness, and itching. This article reviews from different journals
in which developed analytical methods for identification and quantitative determination of
Dexamethasone as a single or combination with other drugs in bulk and pharmaceutical
dosage form. The most commonly used methods for the determination of Dexamethasone
presented in this article are chromatographic methods: HPLC, HPTLC, Uv-Visible
spectrophotometric methods and alternative method like polarographic method were reported.
KEY WORDS :-Dexamethasone Sodium Phosphate, Chromatographic method, Uv visible
method
1) INTRODUCTION:
Dexamethasone Sodium Phosphate [9-Fluoro-11b,17-dihydroxy-16a-methyl-3,20-dioxopregna1,4-dien-21-yl disodium phosphate] is appears as a White Crystalline Powder (Figure 1)(1). The
drug is Freely soluble in water, methanol and slightly soluble in ethanol (96%), practically
insoluble in methylene chloride(2). Dexamethasone Sodium Phosphate has pKa values is 6.00(3)
and melt at 233-235°C(4)
Figure 1: Chemical structures of Dexamethasone Sodium
Phosphate(1)
Dexamethasone is a glucocorticoid agonist. Unbound dexamethasone crosses cell membranes
and binds with high affinity to specific cytoplasmic glucocorticoid receptors. This complex binds
to DNA elements (glucocorticoid response elements) which results in a modification of
transcription and, hence, protein synthesis in order to achieve inhibition of leukocyte infiltration
at the site of inflammation, interference in the function of mediators of inflammatory response,
suppression of humoral immune responses, and reduction in edema or scar tissue. The
antiinflammatory actions of dexamethasone are thought to involve phospholipase A2 inhibitory
proteins, lipocortins, which control the biosynthesis of potent mediators of inflammation such as
prostaglandins and leukotrienes.(5)
2) METHODS FOR THE DETERMINATION OF DEXAMETHASONE SODIUM
PHOSPHATE
a) Compendial Method:
Dexamethasone Sodium Phosphate is official in Indian pharmacopoeia,
British
Pharmacopoeia,
United
State
Pharmacopoeia
and
European Pharmacopoeia for quantitative analysis(table-1)
Table-1 Official compendial methods for assay of dexamethasone Sodium Phosphate
INDIAN PHARMACOPOEIA(1)
1)
Method
Uv Visible Spectrophotometry
Procedure
Weigh drug and dissolve in sufficient water and measure the
absorbance at 240nm.Calculate the content of dexamethasone
sodium phosphate
BRITISH PHARMACOPOEIA(2)
Method
Uv Visible Spectrophotometry
Procedure
Weigh drug and dissolve in sufficient water and measure the
absorbance at 241.5nm. Calculate the content of dexamethasone
sodium phosphate
UNITED STATES PHARMACOPOEIA(6)
Method
Liquid Chromatography
2)
3)
Procedure  Mobile phase :- Use variable mixtures of Solution A and B.
Solution A :- methanol, water, Buffer solution (350:350:300)
Solution B :- methanol and Buffer solution (700:300).
(Buffer solution :- Ammonium acetate dissolve in water and pH 4
adjust with glacial acetic acid)
EUROPEAN PHARMACOPOEIA(7)
4)
Method
Uv Visible Spectrophotometry
Procedure
Weigh drug and dissolve in sufficient water and measure the
absorbance at 241.5nm. Calculate the content of dexamethasone
sodium phosphate
b) Spectrophotometric Method:
There are many spectrophotometric methods reported yet to determine
dexamethasone sodium phosphate as a single and combination with other
drug(table-2).
Table-2 Developed spectroscopic method for Dexamethasone Sodium Phosphate
Sr.
No.
1.
2.
3.
4.
5.
6.
Title
Solvent and
wave length
Development
and
Validation
of
UV- Distilled water,
spectrophotometric Method for the Estimation of 242nm
Dexamethasone Sodium Phosphate in Bulk and
Pharmaceutical Dosage Form
Spectrophotometric Determination of Corticosteroids 780 nm
and its Application in Pharmaceutical Formulation
Ratio Derivative UV Spectroscopy Method for Distilled water,
Simultaneous
Estimation
of
Moxifloxacin 253.60 nm
Hydrochloride
and
Dexamethasone
Sodium
Phosphate in Pharmaceutical Dosage Form
Validated First and Second Order Derivative UV Distilled water,
Spectrophotometric Methods for Simultaneous 241 nm
Estimation of Moxifloxacin Hydrochloride and
Dexamethasone Sodium Phosphate in Ophthalmic
Dosage Form
Simultaneous Estimation of Moxifloxacin
Distilled water,
Hydrochloride and Dexamethasone Sodium
241.6 nm
Phosphate in Bulk and in Eye Drops by UVspectrophotometry
Chemometrics Assisted Spectroscopic Determination
of Vitamin B6, Vitamin B12 and Dexamethasone in
Injectables
Ref.No.
8
9
10
11
12
13
c) Polarographic Method
There is only one polarographic methods reported yet to determine
Dexamethasone Sodium Phosphate(table-3)
Table-3 Developed polarographic method for Dexamethasone Sodium Phosphate
Sr.
No.
1.
Title
solvent
Trace Determination of Dexamethasone Sodium Acetate
Phosphate in Pharmaceutical Formulations
by (pH 5.0)
Differential Pulse Polarography
Ref.No.
buffer 14
d) Chromatographic Methods
There are many chromatographic methods reported yet to determine
dexamethasone sodium phosphate as a single and combination with other
drug(table-4).
Table-4 Developed Chromatographic method for Dexamethasone Sodium Phosphate
Sr.
No.
1.
2.
3.
4.
5.
6.
7.
8.
Title
Analysis of Dexamethasone Sodium Phosphate
Injection and Ophthalmic Solution by HPLC,
Kinetic Interpretation and Determination of
Shelf Life
Separation and Determination of Dexamethasone
Sodium Phosphate in Cochlear Perilymph Fluid
by Liquid Chromatography with Ultraviolet
Monitoring and Electrospray Ionization Mass
Spectrometry Characterization
Determination of Dexamethasone Sodium
Phosphate in the Vitreous by High Performance
Liquid Chromatography
Chemical Stability of Dexamethasone Sodium
Phosphate after Reconstitution in 0.9% Sodium
Chloride Injection and Storage in Polypropylene
Syringes
HPLC-UV
Method
for
Simultaneous
Determination of Ofloxacin and Dexamethasone
Sodium Phosphate in Bulk and Pharmaceutical
Formulations
Simultaneous Determination of Moxifloxacin
Hydrochloride and Dexamethasone Sodium
Phosphate in Eye Drops by HPLC and
Absorbance Correction Method
Simultaneous Estimation of Moxifloxacin
Hydrochloride and Dexamethasone Sodium
Phosphate in Bulk and in Ophthalmic Solution
by RP- HPLC
Development of a Liquid Chromatographic
Method for Ear Drops Containing Neomycin
Sulphate, Polymyxin B Sulphate and
Mobile phase
wavele
ngth
-
Ref.
No.
15
-
Acetonitrile:
Ammonium
acetate(23:77v/v)
245 nm
16
methanol
254 nm
17
278 nm
18
Phosphate buffer(pH 236nm
4):Acetonitrile(50:5
0)
19
Methanol:
Water: 254 nm
Triethylamine
(60:40:0.75)
20
Methanol:
240 nm
Water(75:25 v/v) pH
adjusted to 3.0 with
ortho-phosphoric
acid of aqueous
phase
21
-
22
-
-
9.
10.
11.
12.
13.
14.
15.
Dexamethasone Sodium Phosphate
Simultaneous Determination of Gatifloxacin and
Dexamethasone Sodium Phosphate in Bulk and
Pharmaceutical Formulations by HPLC
Liquid
Chromatographic
Method
for 0.01M
Phosphate
Determination
of
Moxifloxacin
and buffer (pH 6.0) and
Dexamethasone Sodium Phosphate in Eye Drops Acetonitrile (50:50,
v/v)
Simultaneous Determination of Dexamethasone Acetonitrile 5%v/v
Sodium Phosphate and Chloramphenicol in and Glacial acetic
Ophthalmic Solutions
acid(36:64v/v)
Stability Indicating HPLC Method for Phosphate
buffer
Simultaneous Determination of Dexamethasone (pH
6.8)
and
Sodium Phosphate and Chloramphenicol in Bulk Acetonitrile (70:30,
and Formulations
v/v)
Simultaneous Determination of Ciprofloxacin Phosphate
buffer
Hydrochloride and Dexamethasone Sodium (pH
4)
and
Phosphate in Eye Drops by HPLC
Acetonitrile (65:35,
v/v)
Validated HPTLC Method for Simultaneous Chloroform:
Determination of Ofloxacin and Dexamethasone Acetonitrile:
1Sodium Phosphate in Eye Drops
butanol : Formic
acid (3:1:3:3)
Application of a Stability-indicating HPTLC Acetonitrile : Water
Method for Simultaneous Determination of : Ammonia (10:3:0.5
Chloramphenicol and Dexamethasone Sodium v/v/v), pH adjusted
Phosphate in Eye Drop
to 7.8 with 1M Hcl
254 nm
23
254 nm
24
25
254 nm
26
254 nm
27
28
-
262 nm
29
3) DISCUSSION
The presented review highlights on various analytical methods published on Dexamethasone
Sodium Phosphate and combination with other drug.HPLC-UV methods were found to be most
sensitive for Dexamethasone Sodium Phosphate. Various chromatographic conditions are
presented in under Table 4. The HPLC method could be automated; there are different column
fillings; different solvents with different polarity as mobile phases and different detection modes.
The faster time, high sensitivity, specificity and better separation efficiency enable HPLC to be
used frequently for the simultaneous qualitative and quantitative determination of
Dexamethasone Sodium Phosphate in the comparison with the other methods. There is no doubt
on the fact that these chromatographic methods are rapid and far more economical .In this way
various analytical methods for the estimation of these Dexamethasone Sodium Phosphate in bulk
or in various matrixes like plasma, alone or in combination with other drugs is discussed. The
presented information is useful for the researchers especially those involved in the formulation
development and quality control of Dexamethasone Sodium Phosphate and combination with
other drug.
4) REFERENCES:
1) Indian Pharmacopoeia, The Indian Pharmacopoeia Commission Ghaziabad, Govt. of
India Ministry of Health and Family Welfare,vol.II:1175-1176, 2010.
2)
British Pharmacopoeia, The Department of Health, London: The
Office,vol.I:647-649, 2010.
Stationary
3)
Kalia YN, et. al., “Transdermal iontophoresis of dexamethasone sodium phosphate in
vitro and in vivo: Effect of experimental parameters and skin type on drug stability and
transport kinetics”, European Journal of Pharmaceutics and Biopharmaceutics,
2010;75 (2):173-178.
4)
Neil MJ, Smith A., “The Merck Index”, 13th edition, Published by Merck Research
Laboratories,2960, 2001.
5)
http://www.drugbank.ca/drugs/DB01234
6)
The United States Pharmacopoeia (USP 32 NF 27) Asian Edition, Rockville, MD:USP
Convention Inc.,vol.II:2089-2090, 2009.
7)
The European Pharmacopoeia, published by the European Directorate for the Quality
of Medicines & Health Care (EDQM),7th edition, vol.II:1812-1814, 2011.
8)
G.N. Renuka Devi, V. Prathyusha, K. Shanthakumari, S. A. Rahaman, “Development
and Validation of UV-spectrophotometric Method for the Estimation of Dexamethason
Sodium Phosphate in Bulk and Pharmaceutical Dosage Form”, Indo American Journal
of Pharmaceutical Research,2013;3(7):5055-5061.
9)
Singh DK and Verma Rohan, “Spectrophotometric Determination of Corticosteroids
and its Application in Pharmaceutical Formulation”, Iranian Journal of Pharmacology
& Therapeutics, 2008;7(1):61-65.
10) Chothani D., Bhalani J., Vadaliya KR, "Ratio Derivative UV Spectroscopy Method for
Simultaneous Estimation of Moxifloxacin Hydrochloride and Dexamethasone Sodium
Phosphate in Pharmaceutical Dosage Form", Inventi Rapid: Pharm Analysis & Quality
Assurance, 2013;2013(2):1-5.
11) Bhalani J., Vadalia K., Dedania ZR, “Validated First and Second Order Derivative UV
Spectrophotometric Methods for Simultaneous Estimation of Moxifloxacin
Hydrochloride and Dexamethasone Sodium Phosphate in Ophthalmic Dosage Form”,
Inventi Rapid: Pharm Analysis & Quality Assurance, 2012;2012(4):1-5.
12) Dhumal DM, Shirkhedkar AA, Surana SJ, “Simultaneous Estimation of Moxifloxacin
Hydrochloride and Dexamethasone Sodium Phosphate in Bulk and in Eye Drops by
UV-Spectrophotometry”, Analytical Chemistry an Indian Journal, 2013;12(3).
13) Nepote AJ, Damiani PC, Oliviri AC, “Chemometrics assisted spectroscopic
determination of vitamin B6, vitamin B12 and dexamethasone in injectables”, Jornal of
Pharmaceutical and Biomedical Analysis, 2003;31(4):621 627.
14) Jeyaseelan C., and Joshi A., “Trace Determination of Dexamethasone Sodium
Phosphate in Pharmaceutical Formulations by Differential Pulse Polarography”,
Analytical and Bioanalytical Chemistry, 2002;373(8):772-776.
15) A. Ghanbarpour and M. Amini, “Analysis of Dexamethasone Sodium Phosphate
Injection and Ophthalmic Solution by HPLC, Kinetic Interpretation and Determination
of Shelf Life”, Journal of Science, 1995;6(4):226-230.
16) Liu H, et al., “Separation and Determination of Dexamethasone Sodium Phosphate in
Cochlear Perilymph Fluid by Liquid Chromatography with Ultraviolet Monitoring and
Electrospray Ionization Mass Spectrometry Characterization”, Journal of
Chromatography B Analytical Technology Biomedical Life science, 2004;805(2):255260.
17) Kwak H. and D'Amico D., “Determination of Dexamethasone Sodium Phosphate in the
Vitreous by High Performance Liquid Chromatography”, Korean Journal Ophthalmol,
1995;9(2):79-83.
18) Gupta Vishnu D., “Chemical Stability of Dexamethasone Sodium Phosphate after
Reconstitution in 0.9% Sodium Chloride Injection and Storage in Polypropylene
Syringes”, International Journal of Pharmaceutical Compounding, 2002;6(5):395-397.
19) Karanam Sireesha and Katakam Prakash, “HPLC-UV Method for Simultaneous
Determination of Ofloxacin and Dexamethasone Sodium Phosphate in Bulk and
Pharmaceutical Formulations”, International Journal of Pharmacy and Pharmaceutical
Sciences, 2012;4(1):415-418.
20) Dabhi MJ, et al., “Simultaneous Determination of Moxifloxacin Hydrochloride and
Dexamethasone Sodium Phosphate in Eye Drops by HPLC and Absorbance Correction
Method”, Journal of Chemical and Pharmaceutical Research, 2012;4(10):4462-4467.
21) Dhumal DM, Shirkhedkar AA, Nerkar PP, Surana SJ, “Simultaneous Estimation of
Moxifloxacin Hydrochloride and Dexamethasone Sodium Phosphate in Bulk and in
Ophthalmic Solution by RP-HPLC”, Journal of the Chilean Chemical Society,
2012;57(4):1344-1347.
22) Pendela M., Hoogmartens J., Adams E., “Development of a Liquid Chromatographic
Method for Ear Drops Containing Neomycin Sulphate, Polymyxin B Sulphate and
Dexamethasone Sodium Phosphate”, Journal of Pharmaceutical and Biomedical
Analysis, 2004;36(4):751-757.
23) K. Sireesha and K. Prakash, “Simultaneous Determination of Gatifloxacin and
Dexamethasone Sodium Phosphate in Bulk and Pharmaceutical Formulations by
HPLC”, African Journal of Pharmacy and Pharmacology, 2011;5(17):1990-1995.
24) Katakam Prakash and Karanam R. Sireesha, “Liquid Chromatographic Method for
Determination of Moxifloxacin and Dexamethasone Sodium Phosphate in Eye Drops”,
Eurasian Journal of Analytical Chemistry, 2012;7(2):89-95.
25) Shadoul W.A., Gad Kariem E.A., Adam M.E., Ibrahim K.E., “Simultaneous
Determination of Dexamethasone Sodium Phosphate and Chloramphenicol in
Ophthalmic Solutions”, International Journal of Chemical Science and Technology,
2011;1(2):60-69.
26) Katakam Prakash, K.R. Sireesha, Adiki Shantha Kumari , “Stability Indicating HPLC
Method for Simultaneous Determination of Dexamethasone Sodium Phosphate and
Chloramphenicol in Bulk and Formulations” International Journal of Pharmacy and
Pharmaceutical Sciences, 2012;4(4):505-510.
27) Katakam Prakash and Karanam R. Sireesha, “Simultaneous Determination of
Ciprofloxacin Hydrochloride and Dexamethasone Sodium Phosphate in Eye Drops by
HPLC”, Journal of Chemistry, 2012;9(3):1077-1084.
28) Maradiya Jaydeepkumar K, et al., Suhagia Bhanubhai N., Rathod Ishwarsinh S.,
“Validated HPTLC Method for Simultaneous Determination of Ofloxacin and
Dexamethasone Sodium Phosphate in Eye Drops”, World Journal of Pharmacy and
Pharmaceutical Sciences, 2013;2(2):593-600.
29) Seid Yimer, Hymete Araya, Bekhit Adnan A.,“Application of a Stability-indicating
HPTLC Method for Simultaneous Determination of Chloramphenicol and
Dexamethasone Sodium Phosphate in Eye Drop”, Thai Journal of Pharmaceutical
Sciences, 2012;36(3):94.