Non Chiral And Chiral Capillary Zone Electrophoresis Methods For The Analysis Of Fluoroquinolones And Primaquine
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Date
2008-06
Authors
Elbashir, Abdalla Ahmad
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Abstract
A capillary zone electrophoresis (CZE) method has been developed for the
individual determination of the antibiotics gemifloxacin (GEM), lomefloxacin
(LOM), ofloxacin (OFL) and sparfloxacin (SPAR) in tablets. The CZE separation
was performed using a 75 I-Im x 35 cm fused-silica capillary under the following
conditions: 25°C; applied voltage, 1 ~ kV; 25 mM H3P04-NaOH running buffer
(pH 8.5). The detection wavelength was 254 nm. Flumequine was used as
internal standard. The limits of detection (LODs) of GEM, LOM, OFL and SPAR
were estimated to be 2.93, 3.87, 1.24 and 5.38 I-Ig mL-1
, respectively while the
limit of quantitation (LOOs) were 4.91, 8.93, 4.01 and 9.46 I-Ig mL-1
,
respectively. Recoveries ranging from 94.4 - 108.6% were obtained. Excipients
in commercial tablets and degraded products from different stressed conditions
did not interfere in the assay. The method was successfully applied to the
determination of GEM, LOM, OFL and SPAR in pharmaceutical tablets.
A CZE method for the separation of the enantiomers of OFL using
carboxymethyl-J3-cyclodextrin (CM-J3-CD) as chiral selector is also described.
The highest resolution of OFL enantiomers obtained was around 2.8. This was
achieved using tris-citrate buffer (pH 4.5) that contained 3 mg mL-1 CM-J3-CD.
Recoveries between 98.3-103.4 % were obtained when the method was used
to determine the enantiomers of OFL that were spiked to placebos. The
proposed method is fast, sensitive, inexpensive and its usefulness was
demonstrated for the analysis of five pharmaceutical preparations.
CZE methods have also been developed for the separation of the antimalarial
drug primaquine (PO) from its impurity, the positional isomer quinocide (OC).
Different buffer additives such as native cyclodextrins and crown ethers were
evaluated. The use of 18C6 offers slight advantages over f3-CD such as faster
migration times and improved resolution. But nevertheless, elution times of less
5 minutes and resolution of 2-4 were obtained when both additives were used.
2.12 and 2.71% (w/w) of OC were found in pharmaceutical preparations of PO
from two different manufacturers. Possible mechanism that leads to the
successful separation of the isomers is also discussed.
CZE method for the baseline-separation of the enantiomers of PO and OC in
pharmaceutical formulations is also proposed. Optimum separations of the
three components were separated using 50 mM tris phosphate buffer (pH 3.0)
containing 15 mM hydroxypropyl-y-cyclodextrin (HP-y-CD) as background
electrolyte. Under the optimized conditions, the components were successfully
separated in about 5 min. The proposed method was applied for the
determination of OC impurity in PO formulations. The separation of the
enantiomeric pairs of PO and those of OC was also successfully carried out
using a dual chiral selector (15 mM HP-y-CD and 4 mg mL-1 sulphated-p-CD,
pH 4.0), and was operated in the reversed polarity mode.
Description
Keywords
Electrophoresis Methods , For The Analysis Of Fluoroquinolones