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Development and validation of UV-Method for simultaneous estimation of Artesunate and Mefloquine hydrochloride in bulk and marketed formulation Akshay D. Sapakal, Dr. K. A.Wadkar, Dr. S. K. Mohite, Dr. C. S. Magdum

Development and validation of UV-Method for simultaneous estimation of Artesunate and Mefloquine hydrochloride in bulk and marketed formulation Akshay D. Sapakal, Dr. K. A.Wadkar, Dr. S. K. Mohite, Dr. C. S. Magdum

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Published by Habibur Rahman
Scholars Academic Journal of Pharmacy
Scholars Academic Journal of Pharmacy

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Scholars Academic Journal of Pharmacy (SAJP) ISSN 2320-4206
 Sch. Acad. J. Pharm., 2013; 2(4):293-297
©Scholars Academic and Scientific Publisher (An International Publisher for Academic and Scientific Resources)www.saspublisher.com 
293
Research ArticleDevelopment and validation of UV-Method for simultaneous estimation of Artesunate and Mefloquine hydrochloride in bulk and marketed formulation
Akshay D. Sapakal*
1
, Dr. K. A.Wadkar
2
, Dr. S. K. Mohite
1
, Dr. C. S. Magdum
1
 
1
Rajarambapu college of pharmacy, Kasegaon, Tal: Walva, Dist: Sangli- Maharashtra (India).
2
Appasaheb Birnale College of pharmacy, Sangli, Tal & Dist: Sangli- Maharashtra (India).
*Corresponding authorAkshay D.Sapakal
 Email:
Abstract:
A simple, accurate, precise and economical Uv-method for estimation of Artesunate and Mefloquine HCL wasdeveloped. For analysis of Artesunate and Mefloquine HCl, 242nm and 256nm wavelengths were used respectively. Thelinearity range for Artesunate and Mefloquine HCl were 20-140µg/ml & 50-350µg/ml. Results of analysis were validatedstatistically, recovery studies for ART were 98.33-100.33 & for MEF 101.33-101.92. The LOD and LOQ were found to
 be 0.13μg/ml and 0.39μg/m
l for ART. For MEF the LOD and LOQ values were found to be 1.53µg/ml & 2.21µg/ml themethod was validated as per ICH guidelines.
Keywords
: Artesunate, Mefloquine HCL, UV-Spectroscopy.
 
.
INTRODUCTION
ChemicallyART was (3
 R
,5a
,6
 R
,8a
,9
 R
,10
,12
 R
,12a
 R
)- Decahydro-3,6,9-trimethyl-3,12-epoxy-12
 H 
-pyrano[4,3-
 j
]-1,2-benzodioxepin-10-ol, hydrogensuccinate [1] (Fig.1) and chemically MEF was 2- piperidylidyl-2,8-bis (trifluromethyl)-4-quinolinemethanol hydrochloride [2] (Fig.2) both drugs wereactive against
 P.Falciparum and P.vivax
[3-4].
 
Both of drugs were active against the ring stage of the parasite.Artesunate is ideal for the treatment of severe malaria,including cerebral malaria [3-4].Literature survey reveals High PerformanceLiquid Chromatographic (HPLC) [5] , ART and MEFestimation by RP-HPLC method and for determinationof ART in human plasma either as single or incombination with other drugs [6-8]. Colorimetricmethod for estimation of ART is also reported withAmodiaquine [6]. No, method has been reported for simultaneous estimation of both drug by UV-Spectrophotometric method. This paper describes asimple, accurate, sensitive and validated UV-Spectrophotometric method for simultaneousquantification of these compounds as the bulk drug andin combined tablet dosage forms. The proposed methodis optimized and validated as per the InternationalConference on Harmonization (ICH) guidelines [9-10].
Fig.no.1 Chemical structure of ARTFig.no.2 Chemical structure of MEFMATERIAL AND METHODSDrugs and Chemicals
A standard drug samples of ART and MEFwere purchased from Zeal Pharma, Mumbai. Allchemicals and solvents used of AR grade. Marketedformulation Falcigo plus tablet containing ART 100mgand MEF 200mg was used.
Standard stock solution of ART and MEF
An accurately weighed quantity of about 10mg of ART & MEF was taken in 10 ml volumetric flask dissolved in sufficient quantity of methanol and dilutedto 10 ml with the same solvent so as to get the
concentration of 1000 μg/ml.
 
Determination of λ max of ART and MEF
 The standard solution of ART was scanned inthe range of 200-
400 nm and the λ max was found to be
242 nm against methanol. Similarly, the standardsolution of MEF was scanned in the range of 200-400
nm and the λ max was found to be 256 nm against
methanol.
 
Akshay Sapakal
et al.
, Sch. Acad. J. Pharm., 2013; 2(4):293-297
294
Fig.no.3 :
λ max of ART
 Fig.no.4:
λ max of MEF
 Analysis of Marketed formulation
Twenty tablets were weighed accurately; theaverage weight was determined and then triturated to afine powder. A quantity equivalent to 100 mg of ARTand 200 mg of MEF was weighed and transferred to a100 ml volumetric flask containing 70 ml methanol andthe contents were sonicated for 20 min with methanol todissolve the active ingredients. Volume was made up to100 ml with methanol and filtered through Whatmanfilter paper no. 41 to give the stock solution containing
1000 μg/ml of ART and 2000 μg/ml of MEF. Various
dilutions of the tablet stock solutions were scanned andthe absorbances of these solutions were measured at242 nm and 256 nm respectively.
Table No.1: Analysis of Marketed formulation
Drug Label claim% found ±RSD% recovery ±RSDArtesunate 100mg 99.69±0.3297 99.36±0.4183Mefloquinehydrochloride 200mg99.75±0.2345 99.41±0.3214
Method validation
The method was developed and validatedaccording to analytical procedure as per the ICHguidelines [9-10] for validation of analytical proceduresin order to determine linearity, precision, LOD, LOQand accuracy for the analyte .
RESULT AND DISCUSSIONA)
 
LINEARITY
From the standard stock solutions containing1000 µg/ml of ART and 1000 µg/ml of MEF dilutionswere made to prepare range of standard solutionshaving different concentrations of ART (20-140 µg/ml)and MEF (50-350 µg/ml). The absorbances were
measured at 242 nm (λ max of ART) and at 256 nm (λ 
max of MEF) respectively. The results obtained areshown in Table no.2.The linearity of the relationship betweenabsorbances and concentration was determined by plotting the calibration curve for ART and MEFrespectively .The calibration curves are shown in figure2 and 3
Table No.2: Linearity study for ART and MEFSr.no.Conc.
(μg/
ml)Absorbanceof ARTConc.
(μg/
ml)Absorbanceof MEF242nm 256 nm1
20 0.031 50 0.124
2
40 0.035 100 0.233
3
60 0.039 150 0.353
4
80 0.044 200 0.478
5
100 0.049 250 0.607
6
120 0.055 300 0.710
7
140 0.060 350 0.830R=0.9954 R=0.9994
Fig No.5: Calibration curve of Artesunate at 242nmFig.No.6: Calibration curve of Mefloquine at 256nmB)
 
PRECISION
Repeatability of method was established byanalyzing various replicates samples of ART and MEF.Precision was carried out by performing Interday
 
Akshay Sapakal
et al.
, Sch. Acad. J. Pharm., 2013; 2(4):293-297
295variation and intraday variation. In Interday variationthe sample was analyzed on three consecutive days. Inintraday variation the absorbances were measured threetimes in a day.The results for intraday precision are shown inTable no.3 & 4 and for Interday precision are shown inTable no. 5 & 6.
Table No.3: Intraday Precision for ARTConc.
(μg/ml)
 % of label claimMean % of labelclaim± SD %RSDTrial 1 Trial 2 Trial 380
98.44 98.96 99.44 98.94 0.277128 0.28172
100
101.19 100.2 101.19 100.86 0.525389 0.51767
120
98.7 98.57 98.7 98.65 0.075056 0.07686
Table No.4: Intraday Precision for MEFConc.
(μg/ml)
 % of label claimMean % of labelclaim± SD % RSDTrial 1 Trial 2 Trial 3180
99.36 99.85 99.96 99.72 0.319427 0.32032
200
100.06 100.28 100.06 100.13 0.127017 0.12685
220
100.15 99.95 100.28 100.12 0.166233 0.16603
Table No.5: Interday Precision for ART
Conc.(μg/ml)
 % of label claimMean % of labelclaim± SD %RSDDay 1 Day 2 Day 380
99.44 98.96 99.44 99.28 0.277128 0.2939
100
99.23 98.56 98.86 98.88 0.315119 0.3297
120
98.7 98.29 98.7 98.56 0.236714 0.2455
Table No. 6: Interday Precision for MEF
Conc. (μg/ml)
 % of label claimMean % of labelclaim± SD %RSDDay 1 Day 2 Day 3180
99.36 99.85 99.97 99.72 0.32316 0.32406
200
100.06 100.06 100.17 100.09 0.06350 0.06345
220
99.55 99.65 99.85 99.68 0.15275 0.15324

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