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Indian Journal of Pharmaceutical Sciences Scientific Publication of the Indian Pharmaceutical Association Indexed in Ind MED, EMBASE/Excerpta Medica, International Pharmaceutical Abstracts, Chemical Abstracts.
Volume 70
Number 1
January-February 2008
CONTENTS
REVIEW ARTICLES
R. S. KADAM AND K. R. IYER
A Decision Tree for Rapid Quality Assurance and Control of Rifampicin-Containing Oral Dosage Forms for Global Distribution for Tuberculosis Treatment Y. ASHOKRAJ, SHRUTIDEVI AGRAWAL AND R. PANCHAGNULA
K. N. VENUGOPALA AND B. S. JAYASHREE 1-4
Transdermal Delivery by Iontophoresis 5-10
RESEARCH PAPERS In vivo Evaluation of Single Dose Tetanus Toxoid Vaccine Formulation with Chitosan Microspheres R. MANIVANNAN, S. A. DHANARAJ, Y. UDAYA BHASKARA RAO, A. BALASUBRAMANIAM, N. L. GOWRISHANKAR, N. JAWAHAR AND S. JUBIE
94-96
HPLC Estimation of berberine in Tinospora cordifolia and Tinospora sinensis 11-15
G. V. SRINIVASAN, K. P. UNNIKRISHNAN, A. B. REMA SHREE AND INDIRA BALACHANDRAN
96-99
Parenteral Formulation of Zopiclone 16-21
Design and Optimization of Diclofenac Sodium Controlled Release Solid Dispersions by Response Surface Methodology
P. V. SWAMY, P. SUSHMA, G. CHIRAG, K. PRASAD, M. YOUNUS ALI AND S. A. RAJU
99-102
Simultaneous Spectrophotometric Determination of Lansoprazole and Domperidone in Capsule Dosage Form
H. N. SHIVAKUMAR, B. G. DESAI AND G. DESHMUKH
22-30
Evaluation of Free Radical Scavenging Activity of an Ayurvedic Formulation, Panchvalkala
A. P. SHERJE, A. V. KASTURE, K. N. GUJAR AND P. G. YEOLE
31-35
Validation of Different Methods of Preparation of Adhatoda vasica Leaf Juice by QuantiÞcation of Total Alkaloids and Vasicine S. SONI, SHEETAL ANANDJIWALA, G. PATEL AND M. RAJANI
Formulation and Characterization of Mucoadhesive Buccal Films of Glipizide MONA SEMALTY, A. SEMALTY AND G. KUMAR
43-48
Synthesis, Antimicrobial and Anti-inßammatory Activity of 2,5-Disubstituted-1,3,4-oxadiazoles G. NAGALAKSHMI
ASMITA GAJBHIYE, V. MALLAREDDY AND G. ACHAIAH
61-65
P. D. NAKHAT, A. A. KONDAWAR, L. G. RATHI AND P. G. YEOLE 121-124
66-70
S. L. BALDANIA, K. K. BHATT, R. S. MEHTA, D. A. SHAH AND TEJAL R. GANDHI
Optimization of Fast Dissolving Etoricoxib Tablets Prepared by Sublimation Technique D. M. PATEL AND M. M. PATEL
SHORT COMMUNICATIONS Isolation of Liver Aldehyde Oxidase Containing Fractions from Different Animals and Determination of Kinetic Parameters for Benzaldehyde
114-117
Synthesis and Pharmacological Evaluation of (6-Substituted 4-Oxo-4H-chromene-3 yl) methyl N-substituted Aminoacetates 118-120
Development and In Vitro Evaluation of Buccoadhesive Tablets of Metoprolol Tartrate RP-HPLC Estimation of Venlafaxine Hydrochloride in Tablet Dosage Forms
71-76
Simultaneous Estimation of Esomeprazole and Domperidone by UV Spectrophotometric Method
77-84
In Vitro Anthelmintic Activity of Baliospermum montanum Muell. Arg roots
Furosemide-loaded Alginate Microspheres Prepared by Ionic Cross-linking Technique: Morphology and Release Characteristics M. K. DAS AND P. C. SENAPATI
111-113
Effect of Some Clinically Used Proteolytic Enzymes on Inßammation in Rats
56-60
Development and Evaluation of a Chloramphenicol Hypertonic Ophthalmic Solution A. V. JITHAN, C. KRISHNA MOHAN, AND M. VIMALADEVI
V. RAVI, T. M. PRAMOD KUMAR AND SIDDARAMAIAH
A. H. M. VISWANATHA SWAMY AND P A. PATIL
Design and In Vitro Characterization of Buccoadhesive Drug Delivery System of Insulin J. SAHNI, S. RAJ, F. J. AHMAD AND R. K. KHAR
108-111
Novel Colon Targeted Drug Delivery System Using Natural Polymers
49-55
Ascorbic Acid Inhibits Development of Tolerance and Dependence to Opiates in Mice: Possible Glutamatergic or Dopaminergic Modulation S. K. KULKARNI, C. DESHPANDE AND A. DHIR
105-108
Spectrophotometric Estimation of Ethamsylate and Mefenamic Acid from a Binary Mixture by Dual Wavelength and Simultaneous Equation Methods ANJU GOYAL AND I. SINGHVI
36-42
102-105
Novel 2-Pyrazoline Derivatives as Potential Antibacterial and Antifungal Agents SUVARNA KINI AND A. M. GANDHI
SHEETAL ANANDJIWALA, M. S. BAGUL, M. PARABIA AND M. RAJANI
January - February 2008
91-94
Physicochemical and Pharmacokinetic Parameters in Drug Selection and Loading for Transdermal Drug Delivery N. S. CHANDRASHEKAR AND R. H. SHOBHA RANI
Ionic Cross-linked Chitosan Beads for Extended Release of Ciproßoxacin: In vitro Characterization A. SRINATHA, J. K. PANDIT AND S. SINGH
88-91
In vitro Antiviral Activity of some Novel Isatin Derivatives against HCV and SARS-CoV Viruses P. SELVAM, N. MURGESH, M. CHANDRAMOHAN, E. DE CLERCQ, E. KEYAERTS, L. VIJGEN, P. MAES, J. NEYTS AND M. V. RANST
SWATI RAWAT, SUDHA VENGURLEKAR, B. RAKESH, S. JAIN, G. SRIKARTI
85-88
Microwave-Induced Synthesis of Schiff Bases of Aminothiazolyl Bromocoumarins as Antibacterials
S. LAKSHMANA PRABU, A. SHIRWAIKAR, ANNIE SHIRWAIKAR, C. DINESH KUMAR, A. JOSEPH AND R. KUMAR
R. G. MALI AND R. R. WADEKAR
124-128
128-131
131-133
REFEREES FOR INDIAN JOURNAL OF PHARMCEUTICAL SCIENCES DURING 2006 & 2007 134-134
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effective among the synthesized compounds against E. coli, (zone of inhibition 15 mm) and compound P05 was the most effective at 200 μg/ml among the synthesized compounds against P. aeruginosa, ( zone of inhibition 21 mm). At 100 μg/ml the maximum diameter of zone of inhibition (20 mm) against Aspergillus niger was observed for compound P08; indicating that, it is the most effective among the synthesized compounds against Aspergillus niger. The results of the antibacterial and antifungal activity are given in Table 2.
ACKNOWLEDGMENTS The authors are grateful to Shimadzu Analytical Technique Center, Dept. of Chemistry, Pune University, Pune for providing the spectral details in time.
REFERENCES 1. 2.
3.
Mittra AS, Rao S. Synthesis and Fungicidal activity of some 2,4disubstituted thiazoles. Indian J Chem 1977;15:1062-3. 4. Rich S, Horsfall JG. Fungitoxicity of heterocyclic nitrogen compounds. Chem Abst 1952;46:11543. 5. Shah M, Patel P, Korgaokar S, Parekh H. Synthesis of pyrazolines, isoxazoles and cynopyridines as potential antimicrobial agents. Indian J Chem 1996;35:1282-4. 6. Husain MI, Shukla S. Synthesis and Biological activity of 4-(3-Aryl4-oxo-2-thioxothiazolidin-5-ylimino)-3-methyl-1-(N,N-disubstituted amino-methyl)pyrazolin-5-ones. Indian J Chem 1986;25:983-6. 7. Rangari V, Gupta VN, Atal CK. Synthesis, anti-inflammatory and anti-arthritic activity of newer beta-boswellic acid derivatives. Indian J Pharm Sci 1990;52:158-60. 8. Nugent AR, Murphy M, Schlachter TS, Dunn CJ, Smith RJ, Staite ND, et al. Pyrazoline Bisphosphonate esters as novel anti-inßammatory and antiarthritic agents. J Med Chem 1993;36:134-8. 9. Dhar DN. The Chemistry of Chalcones and Related Compounds. New York: Wiley Interscience; 1981. p. 213. 10. Ahmed M, Singh, B, Ranjana Sharma, Talesara GL. Synthesis of 1-(NAlkoxyphthalimido)-3,5-diaryl-2-pyrazolines. Indian J Heterocycl Chem 2004;14:23-5. 11. Collee JG, Miles RS, Watt B. Laboratory control of antimicrobial therapy. In: Collee JG, Fraser AG, Marmion BP, Simmons A, editors. Mackie and McCartney Practical Medical Microbiology, 14th ed. New York: Churchill Livingstone; 1996. p. 151-78.
Fahmy AM, Hassa KM, Khalaf AA, Ahmed, RA. Synthesis of some new beta-lactams, 4-thiazolidinones and pyrazolines. Indian J Chem 1987;26:884-7. Das NB, Mittra AS. Fungicides derived from 2-pyrazolin-5-ones. Indian J Chem 1978;16:638-40.
Accepted 2 February 2008 Revised 4 August 2007 Received 29 May 2006 Indian J. Pharm. Sci., 2008, 70 (1): 105-108
Spectrophotometric Estimation of Ethamsylate and Mefenamic Acid from a Binary Mixture by Dual Wavelength and Simultaneous Equation Methods ANJU GOYAL* AND I. SINGHVI1 Department of Pharmaceutical Chemistry, B. N. P. G. College of Pharmacy, Udaipur - 313 002, 1Department of Pharmaceutical Sciences, M. L. Sukhadia University, Udaipur - 313 001, India
Goyal, et al.: Simultaneous Analysis of Ethamsylate and Mefenamic Acid Two simple, accurate, economical and reproducible spectrophotometric methods for simultaneous estimation of twocomponent drug mixture of ethamsylate and mefenamic acid in combined tablet dosage form have been developed. The first developed method involves formation and solving of simultaneous equation using 287.6 nm and 313.2 nm as two wavelengths. Second developed method is based on two wavelength calculation. Two wavelengths selected for estimation of ethamsylate were 274.4 nm and 301.2 nm while that for mefenamic acid were 304.8 nm and 320.4 nm. Both the developed methods obey Beer’s law in the concentration ranges employed for the respective methods. The results of analysis were validated statistically and by recovery studies. Key words: Ethamsylate, mefenamic acid, simultaneous analysis, two wavelength calculation method, simultaneous equation method *For correspondence E-mail:
[email protected] 108
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Ethamsylate (ESLT) is diethylammonium-2,5dihydroxybenzenesulphonate and is used as a haemostatic agent for prevention and treatment of capillary hemorrhage associated with haemostasis, menorrhagia and post-partum haemorrhage1. The drug is ofÞcial in British Pharmacopoeia with estimation of drug by potentiometric method2. Literature survey reveals that one spectrophotometric 3 and one LC 4 methods are reported for the estimation of ESLT from pharmaceutical formulations. Mefenamic acid (MFNC) is 2-[(2,3-dimethylphenyl) amino]benzoic acid and is used as an analgesic and antiinflammatory agent 5. The drug is official in British Pharmacopoeia with estimation of the drug by non-aqueous titrimetric method6. Literature survey reveals that one spectrophotometric 7, one HPLC8 and three LC9-11 methods have been reported for the estimation of MFNC from pharmaceutical formulations. However none of the methods is yet reported for simultaneous estimation of two drugs from combined pharmaceutical dosage forms. Developed spectrophotometric methods were found to be simple, rapid, accurate, reproducible and economical in comparison to routine extractive or colorimetric methods used for analysis of single drug and have been used successfully for determination of two components from combined tablet dosage form. A PC based Systronic, UV/Vis double beam spectrophotometer (model No. 2101) with spectral bandwidth of 2 nm and wavelength accuracy ±0.5 nm (with automatic wavelength correction) and wavelength readability 0.1 nm increment was employed for all measurements using a matched pair of 10 mm quartz cells. Standard bulk drug samples of ESLT and MFNC were provided by Ochoa Laboratories Pvt. Ltd., New Delhi. Methanol was used as solvent for the preparation of stock solution and for further dilutions. The tablet samples of combined dosage form of ESLT and MFNC [Sylate-M250 (Emcure Pharmaceuticals Ltd., Pune), Sylate-M500 (Emcure Pharmaceuticals Ltd., Pune) and Eklot-MF (Kontest Pharmaceuticals Ltd., Mumbai)] were procured from the local pharmacy. In the Þrst method, pure drug sample of ESLT and MFNC were dissolved separately in methanol so as January - February 2008
to give several dilutions of standard in concentration range of 0-50 μg/ml of each drug. All dilutions were scanned in wavelength range of 200.0 450.0 nm. Two wavelengths selected for formation and solving of simultaneous equation were 287.6 nm and 313.2 nm. Absorptivity coefficient of both the drugs was determined at selected wavelengths. Absorptivity coefficient for ESLT at 287.6 nm and 313.2 nm were 37.40 cm -1g -1 l and 157.78 cm -1g -1 l while respective values for MFNC were 328.80 cm-1g-1 l and 111.62 cm-1g -1 l. Set of two simultaneous equation thus framed were, A1 = 157.78 C1 + 111.62 C2-I and A 2 = 37.40 C 1 + 328.80 C 2 -II, where A 1 and A 2 are absorbance of sample solution at 287.6 nm and 313.2 nm, respectively. C1 and C2 are concentration of ESLT and MFNC, respectively in sample solution in g/l. Validity of above framed equation was checked by preparing Þve mixed standards using pure sample of two drugs, measuring their absorbance at respective wavelengths and calculating concentration of two components. The result of validation studies was found satisfactory. Twenty tablets were accurately weighed and average weight per tablet was determined. Tablets were grounded to Þne powder and tablet powder equivalent to 100 mg ESLT was weighed and extracted four times with 20 ml portions of methanol and filtered through Whatman filter paper no. 41 into a 100 ml volumetric ßask. Washed residue with methanol and added washings to filtrate, volume of filtrate was made to 100 ml mark with methanol. From above filtrate 10 ml was diluted to 100 ml with methanol and finally 1 ml was further diluted to 10 ml with methanol. Absorbance of this final dilution was measured at 287.6 nm and 313.2 nm, respectively, and concentration of two drugs in the sample was calculated using above framed simultaneous equations-I and II. Results of analysis of tablet formulation are reported in Table 1. For method II, set of two wavelengths λ1 (274.4 nm) and λ 2 (301.2 nm) for estimation of ESLT and λ 3 (304.8 nm) and λ4 (320.4 nm) for estimation of MFNC were selected on basis of the principle that absorbance difference between two points on a mixture spectra is directly proportional to concentration of component of interest and independent of interfering component. Five mixed standards of pure drugs containing different concentration of ESLT and MFNC were prepared in methanol. All standards were scanned at
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TABLE 1: RESULTS OF ANALYSIS OF COMMERCIAL FORMULATION Method
Batch
Method I
A B C A B C
Method II
Label claim mg/Tab. ESLT 500 250 250 500 250 250
MFNC 500 250 250 500 250 250
% Label claim estimated* ESLT 100.43 100.74 100.36 99.81 100.73 101.64
MFNC 101.10 100.96 100.90 100.38 101.34 99.42
Standard deviation ESLT 0.6066 0.3524 0.5788 0.9200 0.9170 0.9150
MFNC 0.2586 0.3601 0.1289 0.9585 0.9600 0.9433
% Recovery** ESLT 100.54 101.10 101.22 100.18 100.40 101.86
MFNC 100.78 100.83 101.00 99.86 101.63 99.82
A is Sylate-M500 (Emcure Pharmaceuticals Ltd., Pune), B is Sylate-M250 (Emcure Pharmaceuticals Ltd., Pune) and C is Eklot-MF (Kontest Pharmaceuticals Ltd., Mumbai). ESLT is ethamsylate; MFNC is mefenamic acid. *Each value is an average of Þve estimations; **Average of recovery studies at three different concentration levels.Method I is simultaneous equation method; Method II is two wavelength calculation method
respective set of selected wavelengths. Absorbance difference was measured and respective calibration curve was plotted. Tablet samples were prepared in a similar manner as for method I. Final dilution was analyzed by scanning at respective set of wavelength and absorbance difference values were noted and concentration of ESLT and MFNC was calculated from the respective calibration curve. Results of analysis are reported in Table 1. To study the accuracy, reproducibility and precision for both the developed methods recovery studies were carried out by the addition of standard drug solution to pre-analyzed tablet sample with proper dilutions at three different concentration levels with in the range of linearity for both the drugs. Results of recovery studies were found to be satisfactory and are reported in Table 1. The proposed methods for simultaneous estimation of ESLT and MFNC in combined tablet dosage form were found to be simple, accurate, rapid and economical. The values of recovery were close to 100% indicating reproducibility of the methods. First developed method involving formation and solving of simultaneous equation based on accurate determination of absorptivity coefÞcient of two drugs at two selected wavelengths. Once the equation is framed then it is just required to measure the absorbance of sample solution at selected wavelengths and few calculations that can be manually done. Framed equations were validated using laboratory prepared mixed standards of two drugs which gave satisfactory results.
use of two wavelength calculation so as to remove interference between two components. Proper selection of two wavelengths for estimation of a component is critical. The results of analysis of two drugs from tablet formulation using both the developed methods were found close to 100 percent for both ESLT and MFNC, standard deviation was satisfactorily low indicating accuracy and reproducibility of the methods. Recovery studies were satisfactory which shows that there is no interference of excipients. The developed methods were found to be simple, rapid, accurate and can be used for routine estimation of two drugs from tablet formulations.
ACKNOWLEDGEMENT Authors would like to acknowledge Ochoa Laboratories Pvt. Ltd., New Delhi, India for providing pure drug samples of ESLT and MFNC.
REFERENCES 1. 2. 3. 4.
5. 6. 7.
Second developed method for simultaneous analysis of ESLT and MFNC from combined dosage form make 110
8.
Budavari S, editor. The Merck Index. 13th ed. Whitehouse Station (NJ): Merck and Co Inc; 1997. p. 3757. British Pharmacopoeia, Vol. I, 15th ed. United Kingdom: The HMSO Publication Center; 1998. p. 547. Chitra K, Sujatha K, Ahmed IR, Shalini K, Priya BL, Varghese SS. Spectrophotometric Estimation of Ethamsylate in Tablets and Injection. Indian J Pharm Sci 2005;67:98-100. Nageswara Rao R, Nagaraju P, Sen S, Reddy SV, Radhakrishnamurthy P, Uday Bhaskar S, et al. Determination of Ethamsylate in Pharmaceutical Preparation by Liquid Chromatography. Asian J Chem 2006; 18:783-7. Budavari S, editor. The Merck Index. 13th ed. Whitehouse Station (NJ): Merck and Co Inc; 1997. p. 5820. British Pharmacopoeia, Vol. I, 15th ed. United Kingdom: The HMSO Publication Center; 1998. p. 1105. Vinnykova AV. Spectrophotometric methods for the quantitative determination of mefenamic acid. Farm Zh 1979;3:74-5. Sato J, Owada E, Ito K, Nidya Y, Wakamatsu A, Umetsu M. Simple, rapid and Sensitive reversed phase high performance chromatographic
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method for the determination of mefenamic acid in plasma. J Chromatogr 1989;493:239-43. 9. Poirier JM, Lebot M Cheymol G. Rapid and sensitive liquid chromatographic assay of mefenamic acid in plasma. The Drug Monit 1992;14:322-6. 10. Maron N, Wright C. Application of Photodiode Array UV Detection in the Development of Stability-Indicating LC Methods: Determination of Mefenamic acid. J Pharm Biomed Anal 1990;8:101-5. 11. Rouini MR, Asadipour A, Ardakani YH, Aghdasi F. Liquid Chromatography
Method for Determination of Mefenamic acid in Human Serum. J Chromatogr B Analyt Technol Biomed Life Sci 2004;800:189-92.
Accepted 3 February 2008 Revised 10 August 2007 Received 22 July 2006 Indian J. Pharm. Sci., 2008, 70 (1): 108-111
Novel Colon Targeted Drug Delivery System Using Natural Polymers V. RAVI, T. M. PRAMOD KUMAR* AND SIDDARAMAIAH1 Department of Pharmaceutics, J. S. S College of Pharmacy, S. S Nagar, Mysore - 570 015, 1Department of Polymer Science and Technology, S. J. College of Engineering, Mysore - 570 006, India
Ravi, et al.: Colon targeted drug delivery system A novel colon targeted tablet formulation was developed using pectin as carrier and diltiazem HCl and indomethacin as model drugs. The tablets were coated with inulin followed by shellac and were evaluated for average weight, hardness and coat thickness. In vitro release studies for prepared tablets were carried out for 2 h in pH 1.2 HCl buffer, 3 h in pH 7.4 phosphate buffer and 6 h in simulated colonic fluid. The drug release from the coated systems was monitored using UV/Vis spectroscopy. In vitro studies revealed that the tablets coated with inulin and shellac have limited the drug release in stomach and small intestinal environment and released maximum amount of drug in the colonic environment. The study revealed that polysaccharides as carriers and inulin and shellac as a coating material can be used effectively for colon targeting of both water soluble and insoluble drugs. Key words: Colon targeting, natural polymers, pectin, inulin and shellac
In recent times, colon targeted drug delivery systems have gained importance for the systemic delivery of protein and peptide drugs. This is because the peptide and protein drugs get destroyed or inactivated in acidic environment of the stomach or by pancreatic enzymes in the small intestine 1. Drug targeting to colon is also useful when a delay in drug absorption is desired from therapeutic point of view, such as treatment of diseases that have peak symptoms in the early morning like nocturnal asthma, angina or arthritis2,3. Among the different approaches to achieve colon specific drug delivery, the use of polymers, speciÞcally biodegraded by colonic bacterial enzymes holds promise4,5. The important bacteria present in the colon such as Bacteroides, Bifidobacterium, Eubacterium,
*For correspondence E-mail:
[email protected] January - February 2008
Peptococcus, Lactobacillus, Clostridium secrete a wide range of reductive and hydrolytic enzymes such as β-glucuronidase, β-xylosidase, β-galactosidase, α-arabinosidase, nitroreductase, azoreductase, deaminase and urea hydroxylase. These enzymes are responsible for degradation of di-, tri- and polysaccharides6,7. Pectin is a polysaccharide obtained from plant cell walls. Inulin is a polysaccharide, which is obtained from plants such as onion, garlic, chicory and artichoke. Being soluble in water, pectin is not able to shield its drug load effectively during its passage through the stomach and small intestine. Hence a coat of a considerable thickness is required to protect the drug core in simulated in vivo conditions. The aim of the present study was to develop pectin based matrix tablet with sufÞcient mechanical strength and promising in vitro mouth-to-colon release proÞle. The matrix tablets were coated with inulin and shellac to target the tablets to colon. The coated tablets were evaluated for weight gain, coat thickness and in vitro dissolution studies.
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