Shabnam Pourmoslemi
1, Soroush Mirfakhraee
1, Saeid Yaripour
1, Ali Mohammadi
1,2*1 Department of Drug and Food Control, Faculty of Pharmacy, Tehran University of Medical Sciences, Tehran, Iran
2 Pharmaceutical Quality Assurance Research Center, Faculty of Pharmacy, Tehran University of Medical Sciences, Tehran, Iran
Abstract
Background: A rapid stability-indicating RP-HPLC method for
analysis of doxycycline in the presence of its degradation products was
developed and validated.
Methods:
Forced degradation studies were carried out on
bulk samples and capsule dosage forms of doxycycline using acid, base, H2O2,
heat, and UV light as described by ICH
for stress conditions to demonstrate the stability-indicating power of the
method. Separations were performed on a
Perfectsil® Target ODS column (3-5µm, 125 mm×4 mm), using a mobile phase consisting of methanol-50
mM ammonium acetate buffer (containing 0.1% v/v trifluoroacetic acid and 0.1%
v/v triethylamine, pH 2.5) (50:50 v/v) at room temperature. The
flow rate was 0.8 mL/min.
Results:
The method linearity was investigated in the
range of 25–500 µg/mL (r > 0.9999). The LOD and LOQ were 5 and 25
µg/mL, respectively. The method selectivity was evaluated by peak purity test
using a diode array detector. There was no interference among detection of
doxycycline and its stressed degradation products. Total peak purity numbers were in the range of
0.94-0.99, indicating the homogeneity of DOX peaks.
Conclusion:
These data show the stability-indicating
nature of the method for quality control of doxycycline in bulk samples and capsule
dosage forms.