Skip to main content

Table 2 Validation parameters for determination of IBU, PAP, PAR, PNP, CHZ, and PCA by the proposed methods

From: Impurity profiling of paracetamol toxic impurities in pharmaceutical combination with ibuprofen and chlorzoxazone using HPLC and TLC densitometric methods

Parameter

TLC -Densitometric method

HPLC

IBU

PAP

PAR

PNP

CHZ

PCA

PAP

PAR

PNP

IBU

CHZ

PCA

Range

1–25 μg/band

0.5–20 μg/band

1–25 μg/band

0.5–15 μg/band

1–20 μg/band

0.5–15 μg/band

0.2–10 μg/mL

1–50 μg/mL

0.2–10 μg/ mL

1–50 μg/ mL

1–50 μg/ mL

0.2–10 μg/ mL

Slope 1

− 0.4305

− 0.5606

− 0.8544

− 1.8584

− 1.0469

− 1.7476

288,236

216,766

181,532

117,101

124,914

211,516

Slope 2

23.067

23.027

41.22

48.851

42.19

43.655

Intercept

117.65

62.202

93.693

45.994

64.925

58.266

48,994

29,467

− 7227.6

36,568

2978.7

− 17,423

Standard error of slope 1

0.0171

0.439

0.014

0.659

0.040

0.552

1699.832

1311.307

213.283

525.792

183.375

872.961

Standard error of slope 2

0.462

0.021

0.372

0.040

0.845

0.033

Standard error of intercept

2.237

1.061

2.112

2.102

3.732

1.848

5240.654

39,705.414

1182.038

11,000.36

5091.757

3140.686

Correlation coefficient (r)

0.9997

0.9997

0.9999

0.9998

0.9997

0.9997

0.9999

0.9999

1.0000

0.9999

1.0000

0.9999

LODa

0.32 μg/band

0.15 μg/band

0.17 μg/band

0.14 μg/band

0.29 μg/band

0.14 μg/band

0.06 μg/mL

0.30 μg/mL

0.02 μg/mL

0.31 μg/mL

0.13 μg/mL

0.045 μg/mL

LOQa

0.97 μg/band

0.46 μg/band

0.51 μg/band

0.43 μg/band

0.88 μg/band

0.42 μg/band

0.18 μg/mL

0.89 μg/mL

0.07 μg/mL

0.93 μg/mL

0.41 μg/mL

0.15 μg/mL

Accuracy (R% ± SD)b

99.47 ± 1.07

98.54 ± 1.19

98.62 ± 0.96

98.94 ± 1.12

99.42 ± 0.98

100.04 ± 1.22

99.74 ± 1.04

99.07 ± 1.33

99.33 ± 0.96

99.74 ± 1.12

100.16 ± 0.83

98.02 ± 0.94

Repeatability (RSD %)c

1.41

1.51

1.55

1.36

1.65

1.59

1.39

1.44

1.55

0.97

1.33

1.00

Intermediate precision (RSD %)d

1.77

1.76

1.76

1.81

1.90

1.81

1.53

1.77

1.77

1.38

1.57

1.38

  1. a LOD and LOQ were calculated using the following equations: \(LOD=3.3\upsigma /\text{S}\) and \(LOQ=10\upsigma /\text{S}\) (σ is the residual standard deviation, S is the slope)
  2. b Mean (n = 3) of three concentrations levels covering the specified range
  3. c Intraday (n = 3), three concentrations levels for each compound repeated three times within the same day
  4. d Interday (n = 3), three concentrations levels for each compound repeated three times in three different days