Comparative Purity Study of UV Spectrophotometric and Fourier-Transform Infrared Spectroscopic (FTIR) Techniques for the Determination of Ciprofloxacin Hydrochloride Tablets ty Study of UV Spectrophotometric and Fourier-Transform Infrared Spectroscopic (FTIR) Techniques for the Determination

are It is to the dose within the normal therapeutic range If ciprofloxacin is administered intravenously, plasma concentration profile follows 3-compartment pharmacokinetic model. It is moderately bound (20 to 40%) to plasma proteins and has a large apparent volume of distribution (2 to 3 L/kg). Ciprofloxacin is not readily penetrated Abstract To determine the purity and quality of different brands of ciprofloxacin tablets by using UV spectrophotometry and FTIR spectroscopy as well as provide simple, cost-effective and sensitive spectrophotometric method for determination of ciprofloxacin tablets available in local market, Malaysia. Six different brands of ciprofloxacin tablets were purchased from local market, coded A to F and then analysed by UV spectrophotometry and FTIR spectroscopy. The UV spectrophotometry is based on the absorbance measurement of maximum wavelength of 276nm using distilled water and hydrochloric acid (HCl). All the tablets were evaluated for percentage purity with United State Pharmacopoeia (USP) and British Pharmacopoeia (BP) standards. In FTIR spectroscopy, the spectrum of six different brands of ciprofloxacin tablet were observed and compared among each other. All six ciprofloxacin brands met the specification of weight uniformity. The UV spectrophotometric results using distilled water revealed that two of the market brands are compliance with the official USP limit of 90-110% while only one brand was in the range of 95-105% according to official BP limit. The UV spectrophotometric results using HCl shows that fifty percent of the samples were within the acceptance USP range while four out of six brands fell within the BP specification. The FTIR spectrum of six different brands have the similar characteristic peak corresponding to the functional groups in the chemical structure. FTIR spectroscopy and UV spectrophotometry are developed as simple, quick and cost-effective methods. However, FTIR spectroscopy was more accurate and sensitive and gave better results than UV spectrophotometry [1-62]. The quality and safety of pharmaceutical products are very important.

The oral bioavailability of ciprofloxacin is about 70% to 80%, with minimal loss by first pass metabolism. It is absorbed readily but incompletely. After administration of single oral dose, maximum plasma concentration between 0.28 and 5.92mg/L are achieved within 0.5 to 2 hours. It is increased proportionally to the dose within the normal therapeutic range [11]. If ciprofloxacin is administered intravenously, plasma concentration profile follows 3-compartment pharmacokinetic model. It is moderately bound (20 to 40%) to plasma proteins and has a large apparent volume of distribution (2 to 3 L/kg). Ciprofloxacin is not readily penetrated

ARTICLE INFO Abstract
To determine the purity and quality of different brands of ciprofloxacin tablets by using UV spectrophotometry and FTIR spectroscopy as well as provide simple, cost-effective and sensitive spectrophotometric method for determination of ciprofloxacin tablets available in local market, Malaysia. Six different brands of ciprofloxacin tablets were purchased from local market, coded A to F and then analysed by UV spectrophotometry and FTIR spectroscopy. The UV spectrophotometry is based on the absorbance measurement of maximum wavelength of 276nm using distilled water and hydrochloric acid (HCl). All the tablets were evaluated for percentage purity with United State Pharmacopoeia (USP) and British Pharmacopoeia (BP) standards. In FTIR spectroscopy, the spectrum of six different brands of ciprofloxacin tablet were observed and compared among each other. All six ciprofloxacin brands met the specification of weight uniformity. The UV spectrophotometric results using distilled water revealed that two of the market brands are compliance with the official USP limit of 90-110% while only one brand was in the range of 95-105% according to official BP limit. The UV spectrophotometric results using HCl shows that fifty percent of the samples were within the acceptance USP range while four out of six brands fell within the BP specification. The FTIR spectrum of six different brands have the similar characteristic peak corresponding to the functional groups in the chemical structure. FTIR spectroscopy and UV spectrophotometry are developed as simple, quick and cost-effective methods. However, FTIR spectroscopy was more accurate and sensitive and gave better results than UV spectrophotometry . The quality and safety of pharmaceutical products are very important. ciprofloxacin hydrochloride BP powder was supplied as gift samples from the laboratory of Faculty of Pharmacy, AIMST University for comparison. The powder was manufactured by Aarti Drug Ltd. Maharashtra, India. Its manufacturing license number, batch number, manufacturing date and precaution were also labeled.
Fisherbrand TM analytical balance. UV-VIS spectrophotometer Shimadzu UV-1800 with 1cm path length quartz cells for absorbance measurement [54]. It is connected to the analyzed computer for interpretation and determination of absorbance.

Collection of Different Brands of Ciprofloxacin Tablets
Six different commercially available leading brands of ciprofloxacin tablets, within their shelf life were purchased from various pharmacy outlets in Sungai Petani, Kedah, Malaysia [57,58].
Each brand of ciprofloxacin tablet were labelled to contain 500mg of ciprofloxacin. The ciprofloxacin tablets were blindly named as Brand A, Brand B, Brand C, Brand D, Brand E and Brand F in the present study. The descriptions regarding the brands are shown in (Tables 1 & 2).

Preparation of Crushed Ciprofloxacin Powder
1) 20 tablets of each brands of ciprofloxacin are weighed accurately and the average weight was noted. The percentage deviation of each tablets were also calculated.
2) The powders were kept inside a re-sealable plastic bag to avoid the powder to contact with moisture which may cause the drug to denature.
3) The re-sealable plastic bags were labeled clearly with the name and the crushing date.
4) The plastic bags were kept in desiccator containing silica gel, which is a cool and dry place.

Preparation of Sample and Blank Solution
1) The average weight of each brand was calculated by using the formula below: 2) The sample powders equivalent to 50mg of ciprofloxacin were weighed accurately and transferred into a volumetric flask.
3) 50mg of distilled water was added.
4) The mixture was then stirred for 10 minutes with help of magnetic stirrer and stirring bar. The volume was made up with distilled water (Solution A).

UV Spectrophotometry
The absorbance of ciprofloxacin solution was scanned and measured as a function of wavelength in the 200-400nm UV regions.
The maximum absorption wavelength (λmax) was observed at 276nm and this wavelength was adopted for absorbance measurement. All spectrophotometer measurements were at room temperature laboratory standard.
The absorbance of the resulting Solution C was measured at λmax of 276nm

FTIR Spectroscopy
1) The platinum diamond sampling surface was cleaned before starting measurements of each sample using tissue paper with ethanol and allowed to dry.
2) A fresh background spectrum was measured against air and collected to ensure accuracy of data from samples.
3) Clean crystal check was performed to confirm that the system is ready for measurements [62].

4) Small amounts of finely ground Ciprofloxacin powder
were placed on the diamond sampling crystal and pressed using a clamp to ensure proper contact.
5) The software analysis was performed. The spectrum of each sample was measured over the range of 4000-400cm-1 with spectral resolution 2cm-1. Estimated scan time for spectral acquisition was 25 seconds.
6) The recorded fingerprint spectra of each samples was assessed and peaks were plotted. 7) Characteristic regions of the spectrum were identified and compared among standard and samples.
8) The percentage purity of the peak were calculated by using formula below: Where, Au = absorbance of the sample solution, As = absorbance of the standard solution 2) The percentage purity of six different ciprofloxacin samples was determined by comparing with standard.

Comparison of Percentage Purity of Ciprofloxacin
3) The percentage purity of samples using distilled water as blank solution was compared with that using freshly prepared 0.1 N hydrochloric acid (HCl) as blank solution.
4) The percentage purity of samples by UV spectrophotometric method was compared to that by FTIR spectroscopy.

Results
The average weight of different brands of Ciprofloxacin were calculated and shown in (Tables 3 & 4   Weight of each tablet for different brands (mg)   (Tables 6 & 7).
For ciprofloxacin standard, the percentage purity was found to be 100%. There were 3 trials conducted for each assay of sample. The average percentage purity of sample F was 118.54%.

Measurement of FTIR Spectrum of Different Brands of Ciprofloxacin by FTIR Spectroscopy
( Figure 2) shows the FTIR spectra of ciprofloxacin standard.
The prominent characteristic peaks were found between 3500-    The prominent characteristic peaks were found between 3500-3450cm -1 , which was assigned to stretching vibration of hydroxyl (OH) group and intermolecular hydrogen bonding. Another band at 3000-2950cm -1 represented the alkene and aromatic C-H stretching, especially υ=C-H. The peak at 2900cm -1 was assigned to C-H stretching vibration of cyclopropyl group. The region from 1750 to 1700cm -1 represented the carbonyl C=O stretching. The band at 1650 to 1600cm -1 was assigned to quinolones. (Figure 6) shows the FTIR spectra of ciprofloxacin Brand E. The prominent characteristic peaks were found between 3500-3450cm -1 , which was assigned to stretching vibration of hydroxyl (OH) group and intermolecular hydrogen bonding. Another band at 3000-2950cm -1 represented the alkene and aromatic C-H stretching, especially υ=C-H. The peak at 2900cm -1 was assigned to C-H stretching vibration of cyclopropyl group. The region from 1750 to 1700cm -1 represented the carbonyl C=O stretching. The band at 1650 to 1600cm -1 was assigned to quinolones. (Figure 7) shows the FTIR spectra of ciprofloxacin Brand F. The prominent characteristic peaks were found between 3500-3450cm -1, which was assigned to stretching vibration of hydroxyl (OH) group and intermolecular hydrogen bonding. Another band at 3000-2950cm -1 represented the alkene and aromatic C-H stretching, especially υ=C-H. The peak at 2900cm -1 was assigned to C-H stretching vibration of cyclopropyl group. The region from 1750 to 1700cm -1 represented the carbonyl C=O stretching (Figure 8). The band at 1650 to 1600cm -1 was assigned to quinolones.

Discussion
In this study, the objective were to determine the purity and quality of different brands of ciprofloxacin tablets by using UV spectrophotometry and FTIR spectroscopy as well as provide simple, cost-effective and sensitive spectrophotometric method for determination of ciprofloxacin tablets. Six different marketed brands of ciprofloxacin tablets were purchased. The weight of the tablet is defined as the amount of granules which contains the labeled amount of the active pharmaceutical ingredient. Weight uniformity test is required to assure that the drug content in each unit dose is distributed in a narrow range around the label strength.
If the drug substance forms the greater part of the oral solid dosage form, any weight variation obviously reflects variation in the content of active ingredient [41]. The smaller the weight variation, the better the uniformity of content. The standards for uniformity of weight are applied to tablets, which are supplied in unit dose form as they are subjected to more variations than comparable preparations supplied in multi-dose forms. For tablets with average weight above 250mg, the percentage deviation from the average weight permissible in the official compendium (BP, 2008) is ±5%.
The six different brands of ciprofloxacin met the specification.
However, each two tablets from Brand E and F exceeded the 5% deviation from the average weight, but still conformed to the official compendium specification, which stipulates that not more than two tablets must deviate by 5% from the average weight, if twenty tablets are used for the test.
The occurrence of errors might be due to the presence of tablet fragments or dust on the tablets when weighed, wind from airconditioning, flowing properties of the powder, differences in the bulk densities as well as pressured used and particle size distribution during compression. The UV spectrophotometric method depends on the absorbance measurement of drug at the specific wavelength. It is suitable for the quantitative analysis of ciprofloxacin tablets since it contains suitable chromophore that absorbs radiation in the UV region at the maximum wavelength of 276nm. The maximum wavelength was selected as it can be eliminated the interference from excipients. The distilled water was utilized as a solvent as it is easily available and cheaper than other solvent as well as ciprofloxacin is soluble in hydrochloric acid. The filtration can remove the un-dissolved excipients from ciprofloxacin solution. In the assay UV method using distilled water as blank, the results showed that only Brand C passed the test while other samples fell outside the official BP limit. According to USP, two out of six samples (Brand A and C) fell within the USP limit.
Brand D and E had the percentage purity level below the official stated limit while Brand B and F had the percentage purity level above the upper limit. In contrast to the assay method using HCl as blank, fifty percent of the brands of ciprofloxacin tablet (Brand A, C and F) conformed to the official BP limits of 90-110%. According to USP, four out of six samples (Brand A, B, C and F) had the percentage purity within the stated requirement. On comparing the two solvents used, it was obvious that the assay results using HCl as blank solution was more accurate than that using distilled water.
The reason includes that ciprofloxacin dissolve satisfactorily in HCl rather than in distilled water. The percentage purity might also be affected by factors such as temperature, humidity and light.