TITLE:
An Ultra-sensitive LC Method for the Simultaneous Determination of Paracetamol, Carbamazepine, Losartan and Ciprofloxacin in Bulk Drug, Pharmaceutical Formulation and Human Serum by Programming the Detector
AUTHORS:
Najma Sultana, Muhammad Saeed Arayne, Saeeda Nadir Ali
KEYWORDS:
Paracetamol; Carbamazepine; Losartan; Ciprofloxacin; Time Program
JOURNAL NAME:
American Journal of Analytical Chemistry,
Vol.4 No.1,
January
16,
2013
ABSTRACT:
An ultra-sensitive LC method for the simultaneous
quantitation of paracetamol, carbamazepine, losartan and ciprofloxacin
have been developed and validated following the ICH guidelines at isobestic
point and by programming the detector at individual wavelength of each
component. The components were eluted by 50:50 v/v acetonitrile-water (pH 3.0)
using a Bondapak, C18 (10 μm, 25 × 0.46 cm)
column at flow rate of 1.0 mL·min-1 with
detection wavelength 240 nm at isobestic point and 245, 230, 206 and 272 nm for
paracetamol, carbamazepine, losartan potassium and ciprofloxacin respectively
by programming the detector. Linearity was found to be 0.5 - 24, 0.25 - 8.0, 0.4 - 12 and
0.75 - 10 μg·mL-1 (R2 > 0.999)
with detection limits 99, 20, 30 and 6.0 ng·mL-1 respectively.
Comparison study with time program method showed more sensitivity with
calibration range of 0.4 - 12, 0.2 - 6.0, 0.1 - 3.0 and
0.25 - 8.0 μg·mL-1 (R2 > 0.999)
and LOD values 29, 11, 2.0 and 5.0 ng·mL-1 respectively. Percent
recoveries >98.37% from pharmaceutical formulation and human serum samples
and RSD 2% for inter-day and intra-day assay were obtained. The method was
found to be robust and can be successfully applied for the determination of
studied drugs in, pharmaceutical formulations and human
serum without interference of excipients or endogenous components of serum.