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H.P.L.

C REPORT

NEBIVOLOL

S.NO 1 2 3 4 5 6 7 8 9 10 11 12 13

TEST H.P.L.C CONDITIONS ELUTION A.P.I CONC MOBILE PHASE PH COLUMN WAVE LENGTH FLOW RUNTIME RETENSION TIME AREA TH.PLATES TAILING FACTOR PUMP PRESURE

RESULT ISOCRATIC 10ppm C18 8min 4.637 279992.3 6877.80 0.96

VALIDATION

TEST.1 DAY -1

PRECISSION 1 CONC 30ppm INJECTION AREA 1 710926.0 2 718770.3 3 717463.8 4 717409.9 5 710223.1 6 713762.2 PRECISSION 2 CONC INJECTION 1 2 3 4 5 6

T.P 3539.30 3486.56 3501.24 3502.08 3548.83 3524.69

R.S.D = 0.510

DAY-2

AREA 705473.8 702836.3 702503.7 701658.1 701753.3 701509.8

T.P 3583.34 3598.92 3603.18 3609.18 3609.17 3609.85

R.S.D =0.212

R.S.D. = 0.361

TEST-2

LINEARITY S.NO 1 2 3 4 5

CONC 10ppm 20ppm 30ppm 40ppm 50ppm

AREA 244672.1 452938.4 690648.7 911103.3 1146828.9

INTERCEPT=10494.73 SLOPE C.C =22624.785 = 0.999

GRAPH

Nebivolol
1400000 1200000 a r e a 1000000 800000 600000 400000 200000 0 0 10 20 30 conc. in ppm 40 50 60

TEST-4 TEST-5

L.O.Q L.O.D

0.5ppm 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

that of test results those obtained from standard drug.

System

Suitability System suitability tests were carried out on freshly prepared standard stock solutions of Parameter 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 1 TARGET 2 ADDED 3 TOTAL RECOVERY =99.36 % RECOVERY:-2 FROM LINEARITY CURVE S.NO 1 TARGET 2 ADDED 3 TOTAL RECOVERY =99.16% RECOVERY:-3 FROM LINEARITY CURVE CONC 20ppm 20ppm 40ppm AREA 446655.2 527450.8 963741.8 Th.PLATES 4856.72 4010.40 2949.30 CONC 20ppm 10ppm 30ppm AREA 417588.5 269907.0 685778.7 Th.PLATES 5183.82 7112.57 3714.83

S.NO 1 2 3 RECOVERY = 98.42%

CONC 20ppm 30ppm 50ppm

AREA 411313.1 734732.9 1134482.8

Th.PLATES 5282.69 3372.24 2591.88

AVERAGE RECOVERY = 98.98%

Robustness: S.NO 1 2 3 4 Ruggedness S.NO 1 2 3 4 5 6 RSD Area 690847 694744 694809 698318 698376 693561 0.42 Parameter Standard MP WL PH Change . Area 690648 685951 697996 698008 % Of Change . 0.68 1.06 1.06

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%