Validated high-performance thin-layer chromatographic ... · using FFD design for robustness testing. Therefore, this research paper describes the development of HPTLC method for
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j o u rn a l o f f o o d a nd d r u g an a l y s i s 2 4 ( 2 0 1 6 ) 6 1 0e6 1 9
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Original Article
Validated high-performance thin-layerchromatographic (HPTLC) method for simultaneousdetermination of nadifloxacin, mometasonefuroate, and miconazole nitrate cream usingfractional factorial design
Kalpana G. Patel*, Pratik M. Shah, Purvi A. Shah, Tejal R. Gandhi
Department of Quality Assurance, Anand Pharmacy College, Anand, India
a r t i c l e i n f o
Article history:
Received 14 July 2015
Received in revised form
19 January 2016
Accepted 15 February 2016
Available online 11 April 2016
Keywords:
fractional factorial design
HPTLC
miconazole nitrate
mometasone furoate
nadifloxacin
* Corresponding author. Department of QualE-mail address: kalpanapatel.pharma@gm
j o u r n a l o f f o o d and d ru g an a l y s i s 2 4 ( 2 0 1 6 ) 6 1 0e6 1 9 613
applied on the data of areas of linearity for evaluation of ho-
moscedasticity of variance and deviation from linearity [42].
3Result and discussion
The common detection wavelength selected for analysis was
224 nm as all three drugs were showing optimum response at
224 nm. Mobile phase optimization was carried out in
different solvent systems and different ratios of various sol-
vents were tried such as n-hexane, toluene, methanol, ethyl
Table 2 e Analytical validation parameters of proposed HPTLC
Analytical parameters ND
Calibration rangea (ng/band) 400e2400
Regression equation 4.5482x þ 2460.7
Coefficient of determination (r2) 0.9976
Standard deviation of slope 0.0056
Confidence limit of slopeb 4.55e4.56
Standard deviation of intercept 6.64
Confidence limit of interceptb 2446.59e2460.32
Limit of detection (ng/band) 9.57
Limit of quantification (ng/band) 29.00
Precision study
Repeatabilityc 0.54e1.49
Interday precisionc (d 1) 1.06e1.63
Interday precisionc (d 2) 1.16e1.61
Accuracyc (%) 98.35e99.76
Bartlett's testd(c2) 0.00019
HPTLC ¼ high performance thin layer chromatography; MF ¼ mometasoa Mean of three determinations.b Confidence interval at 95% confidence level and four degree of freedomc n ¼ 3 replicates.d Calculated value c2 less than critical value c2(0.05, 4) ¼ 9.488.
acetate, acetonitrile, diethyl ether, chloroform, and dichloro-
methane. From these, combinations of methanol, ethyl ace-
tate, and toluene gave good results in terms of separation and
therefore, further trials were initiated for different ratios of
methanol, ethyl acetate, and toluene with addition of
different modifiers such as glacial acetic acid, ammonia, for-
mic acid, ortho phosphoric acid, and ammonium formate.
Band characteristic was improved by addition of acetonitrile
to the above mobile phase. However, considerable fronting
was observed in ND, and therefore 3M ammonium formate
was added to minimize fronting. Finally, the mobile phase
method for simultaneous estimation of ND, MF, and MN.
MF MN
100e600 400e2400
7.6661x þ 357.79 3.5916x þ 1285
0.996 0.9964
0.0626 0.0527
7.60e7.73 3.58e3.65
16.35 48.73
340.87e374.68 1234.68e1335.47
7.03 44.77
21.32 135.69
0.37e1.17 0.15e1.14
0.72e1.56 0.95e1.20
0.75e1.65 1.09e1.17
99.36e99.65 99.16e100.25
0.00113 0.003
ne furoate; MN ¼ miconazole nitrate; ND ¼ nadifloxacin.
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