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Table 1 Validation of the method

From: Photodegradation assessment of ciprofloxacin, moxifloxacin, norfloxacin and ofloxacin in the presence of excipients from tablets by UPLC-MS/MS and DSC

Parameter

CIP

MOX

NOR

OFL

RT (min) a

2.52 ± 0.05

3.22 ± 0.05

2.44 ± 0.05

2.47 ± 0.04

Resolution a,b

1.50

0.92

1.51

0.80

LOD (mg mL -1 )

0.06

0.06

0.09

0.10

LOQ (mg mL -1 )

0.18

0.18

0.26

0.30

Linear range (mg mL -1 )

0.18 – 2.00

0.18 – 1.50

0.26 – 2.00

0.30 – 1.50

Regression equation (y):

    

Slope (a ± S a )

139288.9 ± 1140.1

286408.6 ± 3181.1

166591.5 ± 2043.2

284748.3 ± 5341.4

Intercept (b ± S b )

−635.2 ± 1176.9

4474.6 ± 2691.5

−228.6 ± 2067.2

4043.2 ± 4455.5

t = b/S b

0.54 < tα,f statistically insignificant

1.66 < tα,f statistically insignificant

0.11 < tα,f statistically insignificant

0.91 < tα,f statistically insignificant

Normality of residuals c (Shapiro-Wilk test)

0.9343 (p = 0.49)

0.9619 (p = 0.81)

0.9387 (p = 0.54)

0.9462 (p = 0.62)

Correlation coefficient

0.9997

0.9995

0.9994

0.9986

R 2 value

0.9994

0.9989

0.9986

0.9968

Precision (% RSD)

1.04

0.74

1.09

0.64

Intermediate precision (% RSD)

1.30

0.99

1.18

0.80

  1. Regression equation y = ac + b; c - concentration of solution; y- peak area; Sa – standard deviation of slope;Sb - standard deviation of intercept, t- calculated value of Student’s t-test, tα,f =2.776 critical value of Student’s t-test for degrees of freedom f = 4 and significance level α = 0.05;
  2. aMean ± SD (n = 6).
  3. bResolutions were calculated between two adjacent peaks.
  4. c normal distribution of residuals if p > 0.05.