H.P.L.

C REPORT CABERGOLINE

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 Acetonitrile:1%opa:0.025M NaH2PO4 (40:30:30) 2.9 C18 275nm 1.0ml/min 5min 1.655 157841.3 2290.02 1.17 24-27MPa

VALIDATION TEST.1 DAY -1 PRECISSION 1 CONC 15ppm INJECTION AREA 1 209319.8 2 207619.9 3 205102.8 4 208721.3 5 208297.9 6 204610.1

T.P 2032.79 2058.99 2095.80 2039.63 2047.63 2098.82

R.S.D = 0.946

DAY-2

PRECISSION 2 CONC 15ppm INJECTION AREA 1 214743.0 2 212895.0 3 210053.8 4 211177.0 5 210983.4 6 214202.7

T.P 1949.73 1982.17 2021.89 2005.17 2009.65 1962.08

R.S.D = 0.892

R.S.D = 0.919

TEST-2

LINEARITY S.NO 1 2 3 4 5

CONC 5ppm 10ppm 15ppm 20ppm 25ppm

AREA 75313.1 139545.0 212414.4 275380.4 345005.9

INTERCEPT =6965.46 SLOPE = 13504.42 C.C =0.999

Accuracy: conc. =10ppm = 138587.6 139545.0 = 99.31% x 100

GRAPH

cabergoline
400000 350000 300000 a 250000 r 200000 e 150000 a 100000 50000 0 0 5 10 15 conc. in ppm 20 25 30

TEST-4 TEST-5 TEST-6

L.O.Q L.O.D Intermediate Precision Or Ruggedness

1.5ppm 0.4ppm 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 two

Robustness was carried out by varying 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 Parameter

System suitability tests were carried out on freshly prepared standard stock solutions of cabergoline and it was calculated by determining the standard deviation of cabergoline 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 CONC 10ppm 5ppm 15ppm AREA 122987.8 95854.5 218262.0 Th.PLATES 2976.72 2874.41 1893.76

RECOVERY 99.39 %

RECOVERY:-2 FROM LINEARITY CURVE S.NO 1 TARGET 2 ADDED 3 TOTAL CONC 10ppm 10ppm 20ppm AREA 122686.9 153897.3 275480.2 Th.PLATES 2985.92 2360.11 1738.20

RECOVERY - 99.28 % RECOVERY:-3 FROM LINEARITY CURVE S.NO 1 TARGET 2 ADDED 3 TOTAL CONC 10ppm 15ppm 25ppm AREA 138811.9 220402.5 356984.4 Th.PLATES 2643.07 1850.61 1689.51

RECOVERY - 98.98 % AVERAGE RECOVERY =99.21 % Formulation:% of cabergoline in tablet = sample area x std.conc. x tablet avg.wt. x 100

Std. area x sample conc. x lable claim

= 5192 x 5ppm x 5.3mg x 100 75313.1 x 20ppm x 1 mg

=9.99 %