ISSN 1061-9348, Journal of Analytical Chemistry, 2015, Vol. 70, No. 6, pp. 744–746. © Pleiades Publishing, Ltd., 2015.
744
1
Pioglitazone hydrochloride (PGT), a thiazo-
lidinedione class anti-diabetic agent, is chemically
[(±)-5-[[4-[2-(5-ethyl-2-pyridinyl)ethoxy]phenyl]-
methyl]-2,4-] thiazolidine- dione monohydrochlo-
ride [1, 2]. Various analytical methods such as UV-
spectrophotometry [3, 4], liquid chromatography and
micellar electrokinetic chromatography [5–9], high
performance liquid chromatography [10–14] were
reported for estimation of PGT in various matrices
[15, 16]. These reports revealed complex processing
and costly equipment. However, no routine method
has been reported for determination of PGT in differ-
ent dosage forms including transdermal therapeutic
system.
EXPERIMENTAL
Instrumentation. HPLC apparatus (Agilent Tech-
nologies 1120 compact LC system) equipped with a
model LC-20AT pump and SPD 20A variable wave-
length detector and a Rheodyne injection valve with a
20 μL loop was used for development and evaluation
of this method. A Hypersil ODS C-18 (250 × 4.6 mm,
5 μm particle size) was used as separating column.
Data processing was performed with Agilent LC
Ezchrom software.
Drug and chemicals. PGT was obtained from Ran-
baxy laboratories (Gurgaon, Haryana, India) and
marketed drug product Piosys (ONTC Pharmaceuti-
1
The article is published in the original.
cals Ltd., Bangalore, India). Pioz (USV. Ltd., Him-
achal Pradesh, India) was procured from a community
pharmacy. All other reagents were of HPLC grade.
HPLC grade water was prepared using a Milli-Q sys-
tem (Millipore, India).
Method development and validation. The mobile
phase used in the study was a mixture of acetonitrile-
ammonium acetate buffer (pH 5) 60 : 40 (v/v). The
mobile phase was filtered through a 0.45 μm mem-
brane and degassed by sonication for 15 min before
use. The mobile phase was pumped from the solvent
reservoir to the column at a flow rate of 1.0 mL/min
and the volume of the analyte sample injected was
20 μL. The eluents were monitored at 270 nm using
UV-visible detector. All the chromatographic separa-
tions were performed at 25 ± 1°C.
Method validation. The above prepared method
was validated as per International Conference on Har-
monization (ICH) guidelines [17]. The linearity of the
method was determined by diluting the standard stock
solution to 10–100 μg/mL. The dilutions were ana-
lyzed and peak area response against concentration.
Calculated precision was assessed by measurement of
repeatability (intra-day) and intermediate (inter-day)
precision, in accordance with ICH guidelines. Repeat-
ability was studied by assay of six different concentra-
tions of the drug (10, 30 and 50 μg/mL) in one labora-
tory by the same analyst on one working day. Interme-
diate precision was checked by repeating the studies
on three different days.
Validated Reversed Phase HPLC Method for Determination
of Pioglitazone Hydrochloride in Bulk Drug and Tablet Formulations
1
Prem Sunder Prasad, Syed Sarim Imam, Mohammed Aqil*, Mohammad Rizwan,
Yasmin Sultana, and Asgar Ali
Department of Pharmaceutics, Faculty of Pharmacy, Hamdard University M. B. Road New Delhi 110062, India
*e-mail: aqilmalik@yahoo.com
Received November 1, 2013; in final form, July 11, 2014
Abstract—An accurate, sensitive and precise HPLC method was developed and validated for the routine
analysis of pioglitazone hydrochloride in dosage forms. The analyte was chromatographed on a C-18 column
using a mixture of acetonitrile and ammonium acetate buffer (pH 5.0) as mobile phase in ratio 60 : 40 (v/v)
at flow rate 1.0 mL/min. Linearity range was found to be 10–100 μg/mL with a correlation coefficient r
2
=
0.9984. The method was validated for precision, accuracy, robustness, specificity and sensitivity, using bulk
drug samples. Application of method in assay of bulk drug and tablets revealed mean recoveries range from
99.88–100.32%. Due to its simplicity, rapidity, high precision and accuracy, the proposed method may be
used for determining pioglitazone hydrochloride in bulk and dosage forms.
Keywords: pioglitazone, high performance liquid chromatography, tablet formulations
DOI: 10.1134/S106193481506012X
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