H.P.L.

C REPORT

NEBIVOLOL


S.NO TEST RESULT


H.P.L.C CONDITIONS
1 ELUTION ISOCRATIC
2 A.P.I CONC 10ppm
3 MOBILE PHASE
4 PH
5 COLUMN C18
6 WAVE LENGTH
7 FLOW
8 RUNTIME 8min
9 RETENSION TIME 4.637
10 AREA 279992.3
11 TH.PLATES 6877.80
12 TAILING FACTOR 0.96
13 PUMP PRESURE










VALIDATION


TEST.1 PRECISSION 1
CONC 30ppm

DAY -1
INJECTION AREA T.P
1 710926.0 3539.30
2 718770.3 3486.56
3 717463.8 3501.24
4 717409.9 3502.08
5 710223.1 3548.83
6 713762.2 3524.69

R.S.D = 0.510

PRECISSION 2
CONC


DAY-2
INJECTION AREA T.P
1 705473.8 3583.34
2 702836.3 3598.92
3 702503.7 3603.18
4 701658.1 3609.18
5 701753.3 3609.17
6 701509.8 3609.85

R.S.D =0.212

R.S.D. = 0.361






TEST-2 LINEARITY
S.NO CONC AREA
1 10ppm 244672.1
2 20ppm 452938.4
3 30ppm 690648.7
4 40ppm 911103.3
5 50ppm 1146828.9

INTERCEPT=10494.73

SLOPE =22624.785
C.C = 0.999



GRAPH


TEST-4 L.O.Q 0.5ppm
TEST-5 L.O.D 0.15ppm


TEST-6 Intermediate
Precision
Or
Ruggedness
Inter-day variations were performed by using
six replicate injections of standard and sample
solutions of concentrations which were prepared and
analyzed by different analyst on three different days
over a period of one week. Ruggedness also expressed
in terms of percentage relative standard deviation.
TEST-7 Robustness

Robustness was carried out by varying two
parameters from the optimized chromatographic
conditions.
Specificity

The method was determined as specific by
comparing test results obtained from analyses of
sample solution containing excuse ingredients with
0
200000
400000
600000
800000
1000000
1200000
1400000
0 10 20 30 40 50 60
a
r
e
a

conc. in ppm
Nebivolol


that of test results those obtained from standard drug.

System Suitability
Parameter

System suitability tests were carried out on freshly
prepared standard stock solutions of
Nebivolol
and it was calculated by determining the standard
deviation of Nebivolol
standards by injecting standards in five
replicates at 6 minutes interval and the values were
recorded.



RECOVERY:-1
FROM LINEARITY CURVE
S.NO CONC AREA Th.PLATES
1 TARGET 20ppm 417588.5 5183.82
2 ADDED 10ppm 269907.0 7112.57
3 TOTAL 30ppm 685778.7 3714.83

RECOVERY =99.36 %
RECOVERY:-2
FROM LINEARITY CURVE
S.NO CONC AREA Th.PLATES
1 TARGET 20ppm 446655.2 4856.72
2 ADDED 20ppm 527450.8 4010.40
3 TOTAL 40ppm 963741.8 2949.30

RECOVERY =99.16%
RECOVERY:-3
FROM LINEARITY CURVE


S.NO CONC AREA Th.PLATES
1 20ppm 411313.1 5282.69
2 30ppm 734732.9 3372.24
3 50ppm 1134482.8 2591.88

RECOVERY = 98.42%
AVERAGE RECOVERY = 98.98%




Robustness:
S.NO Parameter Change Area % Of Change
1 Standard . 690648 .
2 MP 685951 0.68
3 WL 697996 1.06
4 PH 698008 1.06

Ruggedness
S.NO Area
1 690847
2 694744
3 694809
4 698318
5 698376
6 693561
RSD 0.42


Formulation:-
% of NEBIVOLOL in tablet



= sample area x std.conc. x tablet avg.wt. x 100
Std. area x sample conc. x lable claim

= 55.5 x 30 ppm x 550 mg x 100
690648.7 x 30ppm x 5mg

= 0.88%