A stability-indicating reverse phase high performance liquid chromatography method was developed and

validated for cefixime and linezolid. The wavelength selected for quantitation was 276 nm. The method
has been validated for linearity, accuracy, precision, robustness, limit of detection and limit of quantitation.
Linearity was observed in the concentration range of 2-12 μg/ml for cefixime and 6-36 μg/ml for linezolid.
For RP-HPLC, the separation was achieved by Phenomenex Luna C18 (250×4.6 mm) 5 μm column using
phosphate buffer (pH 7):methanol (60:40 v/v) as mobile phase with flow rate 1 ml/min. The retention time
of cefixime and linezolid were found to be 3.127 min and 11.986 min, respectively. During force
degradation, drug product was exposed to hydrolysis (acid and base hydrolysis), H2O2, thermal
degradation and photo degradation. The % degradation was found to be 10 to 20% for both cefixime and
linezolid in the given condition. The method specifically estimates both the drugs in presence of all the
degradants generated during forced degradation study. The developed methods were simple, specific
and economic, which can be used for simultaneous estimation of cefixime and linezolid in tablet dosage
form.

Diprosalic Lotion is an anti-inflammatory drug product that contains salicylic acid and
betamethasone dipropionate as active pharmaceutical ingredients (APIs). A reversed-phase high
performance liquid chromatography (RP-HPLC) method was developed for simultaneous
determination of salicylic acid, betamethasone dipropionate, and their related compounds in
Diprosalic Lotion. A 150 mm x 4.6 mm I.D. YMC J'sphere ODS-H80 column at 35 degrees C and UV
detection at 240 nm was used. A gradient elution was employed using 0.05% (v/v) methanesulfonic
acid solution and acetonitrile as mobile phases. A total of thirty three compounds from Diprosalic
Lotion samples were separated in 38 min. The stability-indicating capability of this method has been
demonstrated by the adequate separation of all the impurities and degradation products in expired
stability samples of Diprosalic Lotion. The method was validated as per the current ICH guidelines.

A novel stability-indicating reversed phase high performance liquid chromatographic (RP-HPLC)

method for the simultaneous assay of betamethasone-17-valerate, fusidic acid and potassium
sorbate as well as methyl- and propylparaben in a topical cream preparation has been developed. A
100mm×3.0mm ID. Ascentis Express C18 column maintained at 30°C and UV detection at
240nm were used. A gradient programme was employed at a flow-rate of 0.75ml/min. Mobile phase
A comprised of an 83:17 (v/v) mixture of acetonitrile and methanol and mobile phase B of a 10g/l
solution of 85% phosphoric acid in purified water. The method has been validated according to
current International Conference on Harmonisation (ICH) guidelines and applied during formulation
development and stability studies. The procedure has been shown to be stability-indicating for the
topical cream. PMID:24731970

The aim of the present study was the development and subsequent validation of a simple, precise
and stability-indicating reversed phase HPLC method for the simultaneous determination of
guaifenesin, terbutaline sulphate and bromhexine hydrochloride in the presence of their potential
impurities in a single run. The photolytic as well as hydrolytic impurities were detected as 3,5-
dihydroxybenzoic acid, 3,5-dihydroxybenzaldehyde, 1-(3,5-dihydroxyphenyl)-2-[(1,1-dimethylethyl)
amino]-ethanone from terbutaline, 2-methoxyphenol and an unknown impurity identified as (2RS)-3-
(2-hydroxyphenoxy)-propane-1,2-diol from guaifenesin. The chromatographic separation of all the
three active components and their impurities was achieved on Wakosil II column, using phosphate
buffer (pH 3.0) and acetonitrile as mobile phase which was delivered initially in the ratio of 80:20
(v/v) for 18 min, then changed to 60:40 (v/v) for next 12 min, and finally equilibrated back to 80:20
(v/v) for 10 min. Other HPLC parameters were: Flow rate at 1.0 ml/min, detection wavelengths 248
and 280 nm, injection volume 10 μl. The calibration graphs plotted with five concentrations of each
component were linear with a regression coefficient R(2) >0.9999. The limit of detection and limit of
quantitation were estimated for all the five impurities. The established method was then validated for
linearity, precision, accuracy, and specificity and demonstrated to be applicable to the determination
of the active ingredients in commercial and model cough syrup. No interference from the formulation
excipients was observed. These results suggest that this LC method can be used for the
determination of multiple active ingredients and their impurities in a cough and cold syrup.
PMID:22131621

The aim of the present study was the development and subsequent validation of a simple, precise
and stability-indicating reversed phase HPLC method for the simultaneous determination of
guaifenesin, terbutaline sulphate and bromhexine hydrochloride in the presence of their potential
impurities in a single run. The photolytic as well as hydrolytic impurities were detected as 3,5-
dihydroxybenzoic acid, 3,5-dihydroxybenzaldehyde, 1-(3,5-dihydroxyphenyl)-2-[(1,1-dimethylethyl)
amino]-ethanone from terbutaline, 2-methoxyphenol and an unknown impurity identified as (2RS)-3-
(2-hydroxyphenoxy)-propane-1,2-diol from guaifenesin. The chromatographic separation of all the
three active components and their impurities was achieved on Wakosil II column, using phosphate
buffer (pH 3.0) and acetonitrile as mobile phase which was delivered initially in the ratio of 80:20
(v/v) for 18 min, then changed to 60:40 (v/v) for next 12 min, and finally equilibrated back to 80:20
(v/v) for 10 min. Other HPLC parameters were: Flow rate at 1.0 ml/min, detection wavelengths 248
and 280 nm, injection volume 10 μl. The calibration graphs plotted with five concentrations of each
component were linear with a regression coefficient R2 >0.9999. The limit of detection and limit of
quantitation were estimated for all the five impurities. The established method was then validated for
linearity, precision, accuracy, and specificity and demonstrated to be applicable to the determination
of the active ingredients in commercial and model cough syrup. No interference from the formulation
excipients was observed. These results suggest that this LC method can be used for the
determination of multiple active ingredients and their impurities in a cough and cold syrup.
PMID:22131621

An isocratic HPLC method for permethrin determination in raw material and pharmaceutical
presentations as lotion and shampoo has been developed and validated following ICH recommendations.
Cis and trans- isomers, impurities and degradation products are well separated. The chromatographic
analysis were performed on a 4 microm particle C-18 Nova-Pak (Waters, Madrid, Spain) column (15 x
0.39 cm) kept in a Biorad column oven at 35 degrees C. Mobile phase consisted of methanol--water
(78:22, v/v) at a flow rate of 1 ml/min. UV detection was performed at 272 nm and peaks were identified
with retention times as compared with standards and confirmed with characteristic spectra using the
photodiode array detector
Cefixime is an important cephalosporin antibiotic that easily decomposes and releases different related
substances in preparation and storage steps. The objective of the current study was to develop a simple,
precise, and accurate isocratic liquid chromatography (LC) method for the determination of cefixime in the
presence of its related substances generated from thermal stress in the bulk drug. The chromatographic
conditions were comprised of a reversed-phase C18 column (4.6 × 250 mm, 5 μm) with a mobile phase
composed of water: acetonitrile (85:15 v/v, with 0.5% formic acid) and ultraviolet detection (UV). Some
thermal degradation products were identified using a proposed liquid chromatography-mass spectrometry
method. Five peaks (A, B, C, D, and E impurities based on British Pharmacopoeia) were known and a
few unknown peaks appeared in the thermal stress solution of cefixime. The linear regression analysis
data for the calibration plot of the LC-UV method showed a good linear relationship in the concentration
range 0.9-1000.0 μg mL(-1). The recovery of the optimized method was between 94.6 and 98.4% and the
inter- and intra-day relative standard deviations were less than 3.3%. The obtained results shown in the
LC-UV proposed method can be conveniently used in a quality control laboratory for routine analysis of
cefixime for the assay and related substances, as well as for the evaluation of stability samples of bulk
drugs.