ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF TOLPERISONE HYDROCHLORIDE AND DICLOFENAC SODIUM IN BULK AND PHARMACEUTICAL FORMULATION

GPAT courses

Pharma courses

pharma courses

pharma courses



VALIDATION OF THE DERIVATIVE SPECTROSCOPY METHOD
Linearity

The Beer’s law was obeyed. Linear correlation was obtained between D1 absorbance and concentration of DIC (2-10 μg/ml) and TOL (5-25 μg/ml). The linearity of the calibration curve was validated by the value of correlation coefficient of the regression (r). The optical and regression characteristics are listed in Table 3.

Table 3: Optical and regression characteristics (n=3)

Parameter

DIC

TOL

Linearity range (µg/ml)

2-10

5-25

Linearity equation

y = -0.0263x + 0.0108

y = 0.0237x + 0.0077

LOD (µg/ml)

0.1886

0.3111

LOQ (µg/ml)

0.5659

0.9429

Correlation coefficient (r)

0.9973

0.9954

Precision
The % RSD for repeatability of DIC and TOL were found to be 1.8618 and 0.8999 respectively. The value of % RSD for intra-day precision was found to be in the range of 0.93 – 1.06% and inter-day precision was found to be in the range of 1.19 - 1.31%, which indicated that the method was precise.

Table 4 : Repeatability Data (n=6)

Sr. No.

Concentration (µg/ml)

D1 Absorbance

 

DIC

TOL

DIC

TOL

1

6

15

-0.142

0.369

2

6

15

-0.145

0.372

3

6

15

-0.141

0.365

4

6

15

-0.140

0.371

5

6

15

-0.145

0.374

6

6

15

-0.144

0.367

Mean

-0.1428

0.369

SD

0.0021

0.0033

%RSD

1.8618

0.8999

Table 5: Intraday precision data for DIC and TOL

DIC

TOL

Conc

(µg/ml)

D1 Abs

Mean ± S.D. (n=3)

% R.S.D

Conc

(µg/ml)

D1 Abs

Mean ± S.D. (n=3)

%

R.S.D

2

-0.045 ± 0.00057

1.273

5

0.120 ± 0.001

0.8333

6

-0.139 ± 0.0015

1.096

15

0.366 ± 0.0035

0.95778

10

-0.255 ± 0.0030

1.194

25

0.586 ± 0.0045

0.7686

Table 6: Interday precision data for DIC and TOL

DIC

Conc

(µg/ml)

D1 Abs

Mean ± S.D. (n=3)

% R.S.D

2

-0.041 ± 0.00057

1.385

6

-0.142 ± 0.0015

1.073

10

-0.257 ± 0.0035

1.364

Accuracy
The recovery experiments were performed by the standard addition method. The mean recoveries were found to be 99.087 – 100.35 %and 99.93 – 100.46% forDIC and TOL, respectively. The recoveries results indicate that the proposed method is accurate. Results of recovery studies are shown in Table 5 and 6

Table 7: Recovery data of DIC (n = 3)

Level

Sample Conc.
(
µg/ml)

Amt of Drug
added (
µg/ml)

Total Conc.
(
µg/ml)

Amt of Drug recovered (µg/ml)

Recovery

%

Mean ±
SD (%)

%RSD

50%

4

2

6

5.922

98.716

100.35 ± 1.457

1.452

4

2

6

6.091

101.517

4

2

6

6.049

100.817

100%

4

4

8

8.047

100.599

99.401 ± 1.068

1.074

4

4

8

7.883

98.545

4

4

8

7.924

99.059

150%

4

6

10

10.013

100.13

99.087 ± 0.984

0.993

4

6

10

9.895

98.957

4

6

10

9.817

98.174

Table 8: Recovery data of TOL (n = 3)

Sample Conc.
(
µg/ml)

Amt of Drug
added (
µg/ml)

Total Conc.
(
µg/ml)

Amt of Drug recovered (µg/ml)

Recovery

%

Level

Mean ±
SD (%)

%RSD

10

5

15

14.851

99.00

50%

99.93 ± 0.803

0.806

10

5

15

15.054

100.36

 

10

5

15

15.065

100.43

 

10

10

20

20.173

100.86

100%

100.88 ± 1.637

1.623

10

10

 

 


 

Pages

FIND MORE ARTICLES