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ABSTRACT
A simple, precise, selective linear and accurate reverse phase HPLC
method was developed and validated for the assay determination
of Lurasidone in bulk drug and dosage form. Isocratic elution at
flow rate 1.0ml/min was employed on waters XBridge c18
(150x4.6) mm 5m at 30c temperature. The mobile phase
consisted of 0.1% perchloricacid: acetonitrile (50:50) (%v/v). The uv
detection wavelength was 230nm and 10l of sample injected. The
retention time for lurasidone was 5.60min and linearity was
observed in the concentration range of 30-225 g/ml with
correlation coefficient of 0.9999. The percentage relative standard
deviation in accuracy and precision studies was found to be less
than 2%. The method was successfully validated as per
International Conference on Harmonization (ICH) guidelines.
Lurasidone undergoes degradation under acidic, basic, oxidation,
dry heat and photolytic conditions, degradation impurities did not
interfere with the retention time of Lurasidone, and assay method
is thus stability indicating. The method was successfully applied for
routine analysis of lurasidone in bulk drug and dosage form.
Correspondence Author
Pawanjeet J. Chhabda
Department of Biochemistry,
Ahmednagar College, Ahmednagar,
MH,India
Email: pawanjeetvps@rediffmail.com
AU
203.3
231.4
0.05
315. 3
369.8 384.2
0.00
20 0.00
220.00
240.00
260.00
280.00
300.00
320.00
340.00
360.00
380.00
nm
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
(i)
(j)
(k)
P u rit y
A u t o T h re s h o ld
8 0 .0 0
0 .2 2
0 .2 0
0 .1 8
0 .1 6
7 0 .0 0
6 0 .0 0
5 0 .0 0
AU
0 .1 4
4 0 .0 0
0 .1 2
Degrees
0 .2 4
Lurasidone - 5.578
0 .2 6
0 .1 0
3 0 .0 0
0 .0 8
0 .0 6
2 0 .0 0
0 .0 4
1 0 .0 0
0 .0 2
0 .0 0
0 .0 0
- 0 .0 2
5 .3 0
5 .3 5
5 .4 0
5 .4 5
5 .5 0
5 .5 5
5 .6 0
5 .6 5
5 .7 0
5 .7 5
5 .8 0
M in u t e s
5 .8 5
5 .9 0
5 .9 5
6 .0 0
6 .0 5
6 .1 0
6 .1 5
6 .2 0
6 .2 5
6 .3 0
(l)
P u rit y
A u t o T h re s h o ld
4 .0 0
Lurasidone - 5.567
0 .2 2
0 .2 0
0 .1 8
0 .1 6
3 .5 0
3 .0 0
2 .5 0
AU
0 .1 4
0 .1 2
2 .0 0
0 .1 0
Degrees
0 .2 4
1 .5 0
0 .0 8
0 .0 6
1 .0 0
0 .0 4
0 .5 0
0 .0 2
0 .0 0
0 .0 0
- 0 .0 2
5 .3 5
5 .4 0
5 .4 5
5 .5 0
5.55
5 .6 0
5 .6 5
5 .7 0
M in u t e s
5 .7 5
5 .8 0
5 .8 5
5 .9 0
5.95
6 .0 0
6 .0 5
(m)
P u rit y
A u t o T h re s h o ld
9 0 .0 0
Lurasidone - 5.575
0 .2 2
0 .2 0
0 .1 8
0 .1 6
0 .1 4
8 0 .0 0
7 0 .0 0
6 0 .0 0
AU
5 0 .0 0
0 .1 2
4 0 .0 0
0 .1 0
0 .0 8
Degrees
0 .2 4
3 0 .0 0
0 .0 6
2 0 .0 0
0 .0 4
0 .0 2
1 0 .0 0
0 .0 0
0 .0 0
- 0 .0 2
5 .3 0
5 .4 0
5 .5 0
5 .6 0
5 .7 0
5 .8 0
5 .9 0
M in u t e s
6 .0 0
6 .1 0
6 .2 0
6 .3 0
6 .4 0
(n)
3 Typical chromatograms of (a) Blank (b) Standard (c) Sample (d) precision injections (e) Linearity injections
Fig-3
(f) Acid blank (g) Acid sample (h) Base blank (i) Base sample (j) Peroxide blank (k) Peroxide sample (l)Purity plot
of Acid (m) Purity plot of Base (n) Purity plot of Peroxide
16000000
y = 92529x - 12579
R = 0.999
14000000
Mean Area
12000000
10000000
8000000
6000000
4000000
2000000
0
0
50
100
150
Concentration(g/mL)
200
Accuracy
Level
50%
100%
150%
Std
Dev.
%
RSD
0.21
0.21
0.03
0.03
0.05
0.05
Method precision
Intermediate
precision
Set no
Assay (%)
1
2
3
4
5
6
1
2
100.02
100.15
99.78
99.86
100.1
100.24
99.75
100.22
100.34
4
5
6
99.88
99.9
99.55
Stress condition
Mean
assay(%)
Stdev
RSD%
100.03
0.18
0.18
99.94
0.29
0.29
Standard drug
100
Acid degradation
99.57
0.43
Alkali degradation
83.81
16.19
Oxidation degradation
89.81
10.19
Thermal degradation
99.89
0.11
Photolytic degradation
99.90
0.10
Flow
Temperature
%Acetonitrile
variation
Retention
time(min)
USP Tailing
USP Plate
count
0.9ml
6.22
1.37
4235
1.0ml
5.6
1.3
4450
1.1ml
5.01
1.27
4568
25c
5.75
1.34
4325
30c
5.6
1.3
4450
35c
5.25
1.24
4579
45
5.95
1.34
4321
50
5.6
1.3
4450
55
4.98
1.21
4589
6.
7.
ACKNOWLEDGEMENTS
The authors are grateful of M/S GITAM Institute of
Science, GITAM University, Visakhapatnam, India
for providing research facilities.
.
REFERENCES
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with
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liquid
chromatography with tandem mass spectrometr,
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