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et al
Original Article
Exemestane by Rp-
ABSTRACT
A simple, sensitive, precise and Reverse phase high performance liquid chromatographic method has been developed for the quantitative analysis of
Exemestane drug present in drug substance. A suitable HPLC having a isocratic system equipped with manual injector , UV detector is used for this
work. The HPLC separation was achieved on HITACHI L2130 with D Elite 2000 Software with Isocratic with UV-Visible Detector (L-2400).
Develosil ODS HG -5 RP 15cm 4.6 mm 5m particle size and column temperature 25c used as stationary phase. The mobile phase used in this
analysis consists of a mixture of phosphate Buffer (0.01M potassium dihydrogen phosphate & pH adjusted to 2.95 with ortho phosphoric acid ) and
Acetronitrile in a ratio of 30:70. Stock sample is prepared by using acetonitrile and buffer and working sample used is about 100ppm. Flow rate
maintained is about 1.0ml/minute and wave length is about 246nm. Sample colour is Ambient. Injection volume injected about 20L with run time
10 minutes . The proposed method provided linear responses within the concentration range 140ppm for Exemestane . LOD and LOQ values for the
active substance were 0.5 and 1.0 g ml, respectively. Regression equations for the drug substance is about 0.994 in all cases. The precision of the
method was demonstrated using intra-day and inter day assay RSD% values which were in acceptance limit (2%) in all instances. The proposed
method was found to be accurate, precise, reproducible and specific and it can also be used for routine quality control analysis
Key words:
RP-HPLC, Exemestane, method development and validation , acetonitrile , buffer .
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Corresponding Author
T.Mani Manasa *
Samskruti College Of Pharmacy,
Ghatkesar, Hyderabad ,
Telengana, India Hyderabad
Phone: +91- 919618034189
E-mail:tmanumanasa@gmail.com
INTRODUCTION
Exemestane1 is an oral steroidal aromatase inhibitor2
used in the adjuvant treatment of hormonallyresponsive (also called hormone-receptor-positive,
estrogen-responsive) breast cancer in postmenopausal
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Manasa.et al
50
40
30
20
10
8.67
3.33
2.31
Intensity (mV)
Fig 1: EXEMESTANE
0
0
10
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Manasa.et al
70
60
50
40
30
20
10
2.59
2.03
2.23
Intensity (mV)
0
0
10
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Manasa.et al
BASIC DEGRADATION:
PREPARATION OF 0.1N NaOH: 200mg of NaOH
40
2.59
2.24
2.01
0
0
10
3.58
60
20
3.57
Intensity (mV)
80
60
40
10
25
20
15
10
2.59
30
Intensity (mV)
0
0
3.55
35
2.60
2.03
2.25
20
0
0
10
PROCEDURE
3.27
50
40
30
10
2.37
20
2.05
Intensity (mV)
60
0
0
10
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Manasa.et al
RESULTS:
Acid Hydrolysis
(0.1 MHCl)
6Hrs.
99.82
_______
99.82
Basic Hydrolysis
(0.I MNaOH)
6Hrs.
99.32
-----------
98.32
Thermal
600C 1Hr.
Degradation
800C 1Hr.
99.29
-----------
98.29
99.02
______
99.02
1000C 1Hr.
98.93
_____
98.93
Peroxide
6Hrs.
99.69
----------
99.69
UV
1Hr.
99.77
----------
99.77
PRECISION: Repeatability
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Manasa.et al
SYSTEM SUITABILITY:
Exemestane
% interference <0.5 %
Specificity
Range (g/ml)
Linear range
40-140 g/ml
Working range
0.03-100 g/ml
Target range
44,55,60.5 g/ml
Target concentration
55 g/ml
(%Repeatability
Intraday(80,100,120
g/ml)
Inter
g/ml)
100.4,101.0,99.8
0.229
0.22, 0.14, 0.07
LOD (g/ml)
0.5
LOQ (g/ml)
1.0
CONCLUSION
A sensitive& selective RP-HPLC method has been
developed & validated for the analysis of Exemestane
API.Further the proposed RP-HPLC method has
proved for the excellent sensitivity, precision and
reproducibility. The result shows the developed
method is yet another suitable method for assay,
purity & stability which can help in the analysis of
Exemestane in different formulations.
REFERENCES:
1. http://www.drugbank.ca/drugs/DB00990
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