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Journal of computing::quantitative analysis of ciprofloxacin sodium chloride pharmaceutical infusions using ultraviolet-visible spectroscopy
ARPN Journal of Science and Technology
Quantitative Analysis of Ciprofloxacin Sodium Chloride
Pharmaceutical Infusions Using Ultraviolet-visible Spectroscopy
1Affo, W., 2 Mensah-Brown, H., 3 Awuku, J. F., 4 Markwo, A
1, 3, 4 Department of Chemistry, University of Ghana, Legon, Ghana
2 Department of Food Process Engineering University of Ghana, Legon, Ghana
This work was undertaken to develop a rapid and low cost ultraviolet-visible spectrophotometric method for determiningthe amount of ciprofloxacin in ciprofloxacin sodium chloride pharmaceutical infusions. Ultraviolet-visiblespectrophotometric analysis was performed at a pre-determined maximum wavelength of 326 nm with water as diluent and0.018 mg/ml sodium chloride solution as blank. The method was validated for linearity, accuracy, precision andreproducibility. The method was used to estimate the amount of ciprofloxacin in four infusion samples on the Ghanaianmarket. The regression data for the calibration curve exhibited a good linear relationship (R2 = 0.999) having a regressionequation, y =74.554 x + 0.019 over a concentration range of 0.002 - 0.012 mg/ml. The amount of ciprofloxacin in samples
252.1662 mg/100 ml respectively. These concentrations were greater than that indicated on the packs which were 200mg/100 ml for all the samples. When the method was tested with a prepared standard of concentration 0.2 mg/ml, the result
0.0002 representing an increment of 3.4 % more than expected. Hence, the method could
only account for 3.4 % of the increase in the sample concentration. The proposed method gave good validation results andthe statistical analysis performed proved that the method is precise, accurate and reproducible and hence can be employedfor routine analysis of ciprofloxacin in intravenous infusions.
Keywords: Absorbance, ciprofloxacin, fluoroquinolone, ultraviolet-visible spectroscopy
gram-positive bacteria. The gram bacteria are the main
The quinolone antimicrobials embrace a group of
ways of grouping bacteria into two large groups according
synthetic substances that possess a basic nucleus of an N
to their ability to retain the crystal violet dye in gram
alkylated-3-carboxypyrid-4-one ring fused to another
staining protocol or not . Bacteria that retain the dye are
aromatic ring with a substituent on it. The first group of
stained blue or violet and are called gram positive bacteria;
these quinolones surfaced in the 1960’s for treatment
against certain gram negative bacteria. They were
Enterococcus, Bacillus, Clostridium and Listeria [4, 5] .
considered as minor urinary tract disinfectants: an example
Those that are not stained are gram negative, examples are
is nalidixic acid. Further work resulted in the discovery of
Neisseria gonorrhoeae, Neisseria meningitides, Moraxella
the fluoroquinolones which had a fluoro group on position
catarrhalis, Hemophilus influenza, Klebsiella pneumonia,
six of the basic nucleus and were more active biologically
. Fig.1 gives the general structure of fluoroquinoline.
Escherichia coli, Proteus mirabilis, Enterobacter cloacae,Serratia
marcescens, Helicobacter pylori, Salmonella
enteritidis, Salmonella typhi, etc. .
Ciprofloxacin is active against infections that are
caused by most of the above mentioned gram bacteria.
fluoroquinolones are selective against the bacterial enzyme
because the bacterial enzyme is structurally different from
the mammalian enzyme. [7, 8] Ciprofloxacin is used totreat urinary tract infections, typhoid fever, etc. .
General structure of the fluoroquinolones
Ciprofloxacin has no chiral center in its structure as shownin Fig. 2.
Ciprofloxacin chemically is 1-cyclopropyl-6-
quinolinecarboxylic acid . It is a broad spectrumantibacterial agent which belongs to the fluoroquinolone
family. The fluoroquinolones (cinoxacin, ciprofloxacin,nalidixic acid and norfloxacin) act by inhibiting DNAgyrase and thus preventing bacteria DNA replication.
These chemotherapeutic agents are used particularly in
Structure of Ciprofloxacin
ARPN Journal of Science and Technology
Intravenous ciprofloxacin is most frequently
ciprofloxacin in the Aldrich Chemical Catalogue. The
associated with side effects such as nausea, diarrhea,
melting point of the crystalline material was also obtained.
central nervous system disturbance, infusion site reactions,hepatic enzyme abnormalities, eosinophilia, headache,
2.2 Stock Preparation
restlessness, and rash. The majority of these effects are of
A stock solution of concentration 0.05 mg/ml was
mild to moderate severity. An overdose of ciprofloxacin
prepared by first dissolving 0.02 g of crystalline
can lead to the following effects: headaches, dizziness,
ciprofloxacin hydrochloride with 10 ml of distilled water in
drowsiness, disorientation, slurred speech, tremors, nausea
a 100 ml beaker. The resulting solution was then
and vomiting, diarrhea, abdominal (stomach) pain, kidney
transferred quantitatively into a 100 ml volumetric flask,
swirled for complete dissolution and topped to the markwith distilled water. A 25 ml aliquot of this solution was
A variety of analytical methods have been
taken into another 100 ml volumetric flask, topped to the
developed for the analysis of drugs of the 4-quinolones
mark with distilled water, corked and labeled stock A. The
, some of which are High Performance Liquid
procedure was repeated to obtain stock B.
Chromatography (HPLC) recommended by the Britishpharmacopoeia , High Performance Thin Layer
2.3 Preparation of Standards
Standard solutions of concentrations ranging from
Atomic Absorption Spectrometry (AAS). These methods
0.002 mg/ml to 0.012 mg/ml at intervals of 0.002 mg/ml
are expensive and mostly unavailable in many laboratories
were prepared. From each of the stock, 2 ml, 4 ml, 6 ml, 8
in developing countries including Ghana.
ml, 10 ml and 12 ml were taken into separate 50 mlvolumetric flasks using a 10 ml graduated pipette and
There is, therefore, the need to develop a method
topped to the mark with distilled water. These were corked
that is less expensive and with equipment that is widely
and labeled A1 – A6
and B1 – B6
to obtain two sets of
available. Ultraviolet-visible spectroscopy was considered
standards from the respective stock.
and it is one method that is less expensive, easily availableand effective for analyzing drugs belonging to the
2.4 Preparation of the Sample
quinolone group. It involves absorption of radiation in the
Four brands of ciprofloxacin sodium chloride
range of 200 nm to 800 nm within the electromagnetic
pharmaceutical infusions were obtained from various
spectrum . Absorption occurs at a specific part of the
pharmacies in Accra. Sample solutions of concentration
molecule - the chromophore and absorption is highest at
0.004 mg/ml were prepared. A 20 ml aliquot of the drug
the maximum wavelength of 326 nm . Absorption that
sample was transferred into a 100 ml volumetric flask and
leads to electronic transitions from non-bonding (n) to pi-
topped to the mark with distilled water. A 1 ml aliquot of
antibonding (π*) and from pi-bonding (π) to π* are of great
the resulting solution was taken into another 100 ml
diagnostic value in the ultraviolet-visible region.
volumetric flask and distilled water added to the mark.
Ultraviolet-visible spectroscopy has been better applied inassaying than identification, especially in research. The
2.5 Blank Preparation
amount of metals in certain sample substances can bedetermined by this method. This principle is also applied in
I. Sample blank
drug metabolites, where samples are taken from various
Sodium chloride solution with a concentration of
sites of the body and analyzed to determine the amount of
0.018 mg/ml was prepared as sample blank- by dissolving
metabolites at those sites. In reactions leading to the
0.4500 g of sodium chloride with 10 ml of distilled water
formation of products that can absorb within the UV-
in a 50 ml beaker. The resulting solution was transferred
visible region, UV-visible spectroscopy can be used to
into a 50 ml volumetric flask and topped to the mark with
distilled water. A 10 ml aliquot of the resulting solutionwas taken into a 50 ml volumetric flask and distilled water
The objective of this study is to employ UV-
added to the mark. Finally, 0.5 ml of this solution was
visible spectroscopic methods to develop an accurate,
taken into another 50 ml volumetric flask and topped to the
precise, reproducible and economic routine method for the
mark with distilled water. It was corked and labeled sample
estimation of ciprofloxacin intravenous infusions on the
2. MATERIALS AND METHODS
Distilled water was used as blank for the
2.1 Purity and Identification Test
All solutions prepared were used within twelve
Crystalline ciprofloxacin was obtained and its
purity checked. Thin layer chromatography (TLC) analysiswas carried out using silica plates with a mixture ofmethanol, chloroform, ammonia and hexane in ratios: 35
2.6 Measurement of Absorbance
%: 43 %: 17 %: 5 % v/v respectively as the eluent and
spectrophotometer was used for the measurement of
developed with iodine vapour. Infra-red (IR) spectrum of
absorbance. The equipment was warmed for 5 minutes,
the material was superimposable with the spectrum of
ARPN Journal of Science and Technology
after which a wavelength scan was done to obtain thewavelength of maximum absorption. The wavelength of
From the absorbance of the samples, their
maximum absorption obtained was 326 nm. The
corresponding concentrations were interpolated from the
spectrophotometer was then set to a single wavelength
calibration curve and subjected to mathematical and
mode, which is 326 nm. The spectrophotometer was zeroed
statistical calculations to obtain the concentration of the
using distilled water. The cuvette was rinsed and filled with
samples analyzed as well as the associated error. Table 4
standard A1 and the absorbance recorded. This was
below shows the concentrations of the samples with their
repeated for the remaining standards A2 - A6 and B1 - B6.
corresponding expiry date and manufacturer’s specified
The cuvette was rinsed with methanol followed by distilled
concentration, and experimental concentrations of the
water in-between measurements. The cuvette was then
rinsed and filled with the first sample prepared from theciprofloxacin sodium chloride pharmaceutical infusion and
absorbance taken. The absorbance of all the samples
including the sample blank (0.018 mg/ml sodium chloride)
obtained showed a single spot on TLC, with an Rf value of
0.48. The melting point was found to be 254 - 256 °C(literature value 255 – 257 °C). The IR spectrum was
2.7 Data Analysis
identical to that of ciprofloxacin in the Aldrich Chemical
The data obtained for the standards were taken
Catalogue. A calibration curve Eq. (1) (Fig. 1); with a
through mathematical calculations to obtain their
corresponding regression coefficient R2 = 0.999 was
respective concentrations. The concentrations together with
obtained with high linearity which conformed to the Beer-
their corresponding absorbance were taken through least
Lamberts’ law and this also conformed to the specification
square analysis (Skoog et al
., 2004) to obtain the least
of the United States pharmacopoeia. The sodium chloride
square line for the calibration curve given in Fig. 3 and
used in this study had some level of absorption (0.001),
represented by Eq. (1). All associated errors of the samples
which was factored in the calculation and it is necessary to
consider such compounds in similar experiments.
Ciprofloxacin sodium chloride pharmaceutical
infusions from four different manufacturing companies
is absorbance and x
is concentration of
sold on the Ghanaian market were sampled. The samples
were labeled A - D. The concentrations of all the samplesanalyzed were greater than that specified by themanufacturers. On validating the method with a standardsolution of 0.2 mg/ml ciprofloxacin, an increase of 3.4 %was observed whilst the sample concentration gave anaverage increment of 22.5 %. This implies that the methodcan only account for 3.4 % of this increment and theremaining attributed to the content of the drug.
The proposed UV-visible spectrophotometric
reproducible and highly sensitive for the analysis ofciprofloxacin. Therefore, it can be used routinely for the
Calibration curve for ciprofloxacin
determination of ciprofloxacin in ciprofloxacin-basedpharmaceutical formulations on the Ghanaian market.
3.1 Purity and Identity Analysis
To use the crystalline ciprofloxacin material for
Lemke, T. L., Williams, D. A., Roche, V. F.,Zito S.
the calibration curve it was necessary to determine its
W., (2008). Foye’s Principle of Medicinal
purity and identity. The observed melting point was 254 -
Chemistry, 6th Ed., Lippincott Williams and
256 ˚C. The thin-layer chromatography (TLC) analysis
Wilkins: A Wolters Kluwer Business, Philadelphia,
showed a single spot with an Rf value of 0.48. The IR
spectrum of the crystalline material was superimposablewith the IR spectrum of the ciprofloxacin in the Aldrich
Bhalerao, S.R., Rote, A.R., (2012). Application of
Chemical Catalogue. Table 1 gives prominent peaks in
UV spectrophotometric methods for estimation of
ciprofloxacin, whereas Table 2 and Table 3 give the
ciprofloxacin and tinidazole in combined tablet
dosage form, International Journal of Pharmacy and
ciprofloxacin material and ciprofloxacin sodium chloride
Pharmaceutical Sciences, vol. 4 (3), pp. 464-467.
pharmaceutical infusion samples respectively.
ARPN Journal of Science and Technology
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Prominent Peaks in Ciprofloxacin
Peaks ( cm-1)
Absorbance Of Standards Prepared From Crystalline Ciprofloxacin Material
ARPN Journal of Science and Technology
Absorbance Of Ciprofloxacin Sodium Chloride Pharmaceutical Infusion Samples
Manufacturer’s Specified Concentration And Experimental Concentration Data
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ASCO Breast: Implants May Quell Hormone Deficiency By Charles Bankhead, Staff Writer, MedPage Today Reviewed by Dori F. Zaleznik, MD; Associate Clinical Professor of Medicine, Harvard Medical School, Boston. October 04, 2010 MedPage Today Action Points Note that this study was published as an abstract and presented at aconference. These data and conclusions should be considered