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Validation of Uv Spectrophotomeric Method for the Determination of Venlafaxine_78_ijpir_105_10

Validation of Uv Spectrophotomeric Method for the Determination of Venlafaxine_78_ijpir_105_10

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28
Int. J. Pharm & Ind. Res Vol 01 Issue 01 Jan - Mar 2011
 
Original Article 
DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMERICMETHOD FOR THE DETERMINATION OF VENLAFAXINEHYDROCHOLORIDE IN BULK AND SOLID DOSAGE FORMS
*
Sundaraganapathy R, Jambulingam M, Ananda Thangadurai S, Subasini U
Swamy Vivekanandha College of Pharmacy, Tiruchengode, Tamil Nadu, India-637 205.
Introduction
 
Venlafaxine hydrochloride is an anti-depressant agent andchemically it is a cyclohexanol hydrochloride derivative. ItsIUPAC name is [R/S]-1-[2-dimethylamine)-1-[4-Methoxyphenyl)ethyl] cyclohexanol hydrochloride or (+)-1-[2-[(dimethylamino)methyl]p-Methoxybenzyl] cyclohexanolhydrochloride. Venlafaxine is official drug in BritishPharmacopoeia
[1-3]
. HPLC measurements of Venlafaxine ando-desmethyl venlafaxine in human plasma for itsdetermination in pharmaceutical preparations when presentalone. HPLC methods were reported for the estimation ofVenlafaxine dosage forms
[4]
. The review of literaturerevealed that no method is reported for the Venlafaxinehydrochloride in fixed dosage products by UV-spectroscopy.The present paper describes a simple, rapid, accurate andreproducible method for the estimation of Venlafaxinehydrochloride in tablet formulation by first order derivativespectrophotometry.
Materials and Methods:
 Materials
Venlafaxine hydrochloride was a gift sample from LeePharma Pvt. Ltd, Hyderabad. The commercial fixed doseproduct VENLOR 37.5mg and DALIUM 37.5mg wasprocured from the local market.
Equipments
PERKIN ELMER UV-Visible spectrophotometer Lamda 25 with
*Author for Correspondence: 
Prof. R. Sundaraganapathy,Department of Pharmaceutical Chemistry,Swamy Vivekanandha College of Pharmacy,Tiruchengode, India-637 205.Email: sgp.ram@hotmail.com1cm matched quartz cell was used for the measurement ofabsorbance. SHIMADZU-AX-200 electronic balance wasused for weighing the samples. Class-A volumetric glasswares were used
Development of the method
The solution of Venlafaxine was prepared in distilled waterat th
e concentration of 10µg/ml. This was scanned in the
wavelength range of 200-400 nm. Data were recorded atan interval of 5nm. The wavelength selected for Venlafaxinehydrochloride analysis was 224 nm. The spectral data of thedrug shown in Fig 1
 Fig 1:
 
Absorption Spectral data (at 224nm)
-0.100.10.20.30.40.5195 215 235 255 275 295 315 335
 
Analysis of Marketed Formulation
20 tablets were weighed accurately and powdered. Eachcontaining of 37.5 mg quantity equivalent to 10 mg ofVenlafaxine hydrochloride was weighed and dissolved in100ml distilled water. The solution was filtered throughwhatmann filter paper No: 41. Further dilution was made upto 100ml with distilled water in volumetric flask. To set the
theoretical concentration of the drug was 10µg/ml and the
concentration of the drug was determined. The data wasshown in Table 1.
Abstract
Determination of Venlafaxine Hydrochloride in a fixed dosage form was carried out by UV Spectrophotometricmethod. The absorbance values were observed for different dilutions of drug at 224nm and which are used for theestimation of drug without mutual interference of excipients. The solvent used for the dilution is Distilled water. This methodobeys Beer’s Lambert’s law in the concentration range of 2-
14 µg/ml. The results of analysis have been validated
statistically and the recovery studies confirmed the accuracy of this proposed method.
Key words
:
Venlafaxine Hydrochloride, UV Spectrophotometer, Recovery studies.
Wave Length
   A   b  s  o  r   b  a  n  c  e
 
29
Int. J. Pharm & Ind. Res Vol 01 Issue 01 Jan - Mar 2011
 
Table 1: Analysis of Formulation
S. No. Brand Name Amount of drug
(in mg)
% Labelled claimLabelled Estimated
1 VENLOR[Cipla]37.5 36 96.262 DALIUM[Npil]37.5 36 96.26
Validation MethodsLinearity
Standard stock solution was prepared by dissolving 100 mgof each standard drug sample in 100 ml volumetric flaskseparately and the volume was made up with distilled water
 [5].
To get a concentration of 1mg/ml, from this suitabledilution was made in distilled water to get the workingstandard solution of 2-
14 µg/ml for Venlafaxine. The
absorbance was measured at 224 nm
[6]
.
 
For Venlafaxinehydrochloride seven replicated analysis were carried out.Absorbance Vs concentration were plotted to obtain thecalibration graph. The drug obeyed to the Beer’s law to theabove concentration range with R
2
value 0.995836
 
(Table 2& Fig 2).
 Table 2: Linearity
S.No. Concentration Absorbance at 224 nm
1 2 0.04992 4 0.09903 6 0.14984 8 0.19865 10 0.24096 12 0.29017 14 0.3422
Fig 2: Beer’s Law Plot
00.050.10.150.20.250.30.350.40 2 4 6 8 10 12 14 16
 
Precision
Precision is the degree of aggregate among individual testresults when a method is applied repeat ably to multiplesampling of a homogenous sample is known as precision ofthe analytical method.
[7]
Repeatability
Repeatability studies were done by repeatedly observing
the standard solution containing 10 µg/ml of Venlafaxine
hydrochloride % RSD (percentage relative standarddeviation) was calculated and the data was shown in Table3.
 Table 3: Repeatability
Venlafaxine hydrochlorideS.No.Concentration
(g/ml)
Absorbance % RSD
1 1.1282 1.138310 g/ml1.141 0.0054 1.1495 1.1546 1.159
Average of Six Determinations
Inter day
Inter day precision was found out by preparing 10
g/mlequivalent concentration of formulation for three days andstandard deviation was calculated
[8]
. The peak area and %RSD (percentage relative standard deviation) are shown inTable 4.
Table 4: Interday
Day/DateVenlafaxine hydrochloride (10
g/ml)Absorbance % RSD
1
st
day(16.03.2009)1.1221.2351.2470.392
nd
day(17.03.2009)1.2351.1211.2460.393
rd
day(18.03.2009)1.1251.2371.2490.38
Average of three determinations
Intra day precision
Intra day precision was found out by preparing 10
g/mlequivalent concentration of Venlafaxine hydrochloride in theformulation for six times on the same day. The absorbanceof solution was noted and the concentration correspondingwas calculated
[9]
. The data was presented in Table 5.
Table 5: Intraday
S.No.Sample concentration
(
g/ml)
 DrugAbsorbance% RSD
12345610
g/mlVenlafaxineHydrochloride1.1181.2321.3591.2461.3891.4510.62
Average of six determinations
Accuracy and Recovery studies
The accuracy of the experiment was established by usingrecovery studies, ie, by external dilution method. The knownamount of standard was added at 3 different levels of 80%, 100 % and 120 % of samples
[10]
. The result of recoveryanalysis was presented in Table 6.
 
   A   b  s  o  r   b  a  n  c  e
Concentration of Drug in µg/ml
 Y=1.971476e-0.2+2.365571e-0.2*X
 
Correlation co-efficient=0.985836
 
30
Int. J. Pharm & Ind. Res Vol 01 Issue 01 Jan - Mar 2011
 
Table 6: Accuracy and Recovery studies
S.No. Brand Name Wt. of Std Drugadded (
mg)
 Wt. of PowderedTablet
(mg)
 Test Absorbance Content of Drug in percentage PowderedTablet (
mg)
 % Average Content
(mg)
 
1234VENLOR[Cipla]2101112131.9231.9461.9141.95995.4896.6195.0297.28
 
96.091234DALIUM[Npil]2101112131.9481.9611.9261.87696.897.495.693.5
 
95.83
Average of four determinations
Ruggedness
The ruggedness of the UV spectroscopy method wasevaluated by difference in the absorbance and consistentusing a standard working solution. Small differences in theabsorbance and good constancy were observed after threedays. An RSD of less than 0.06% were obtained.The comparable absorbance obtained on different daysindicates that the method is capable of producing resultswith high precision on different days
[11]
.The high degrees of reproducibility of absorbance indicatethat the method is fairly rugged and given in Table 7.
 Table 7: Ruggedness
 
Average of four determinations
Stability
The sample was subjected for stability studies under roomtemperature. Stabilities were studied by performingexperiment to check the changes the absorbance with thefreshly prepared standarad solution
[12]
.
 
The solution underroom temperature was stable upto 5hrs. The data wasshown in
 
Table 8.
 Table 8: Stability
S.No.` Time
(in hrs)
Venlafaxine Hydrochloride % RSDConcentration (
g/ml)
 Absorbance
12345
 
1hrs2 hrs3 hrs4 hrs5 hrs
 
10
g/ml1.1181.1171.1151.1201.112
 
0.0023
Average of five determinations
Results and Discussion
The UV spectrum of Venlafaxine
 
hydrochloride wasobtained by using distilled water as a solvent and thenvalidated. The wave length was found to be 224 nm andlinearity obtained at the concentration range 2-
14 µg/ml
for both bulk and solid dosage forms Fig. 1 shows
Venlafaxine hydrochloride at a concentration of 10 µg/ml is
evident that Venlafaxine hydrochloride shows absorbance atany of these wavelengths could be used for the estimation ofVenlafaxine hydrochloride. The wavelength 224 nm wasselected because it showed maximum absorbance by thesolvent distilled water.The absorption in first derivative mode of Venlafaxinehydrochloride at selected wavelength at 224nm was linearin concentration range of 2-
14 µg/ml. the R
2
was found tobe 0.995836.The percentage recovery varied from 100-103 % w/w forVenlafaxine hydrochloride. The stability absorbance wasmeasured in derivative mode at 224 nm for Venlafaxinehydrochloride at periodic intervals. There was no change inthe absorbance at the wavelength up to 5 hours, indicatingthat the solution was stable for at least 5 hours. Commercialformulation containing Venlafaxine hydrochloride wasanalyzed by proposed method. Analysis of formulation wascarried out. The content of the Venlafaxine was found to be36 mg per tablet. The corresponding standard deviationwas found to be 0.005 for Venlafaxine hydrochloride,indicating that the method has required precision. Theaccuracy of the method was determined by recovery studies.Venlafaxine hydrochloride was determined by recoverystudies were carried out. The recovery was from 100-103%, indicating that the method has required accuracy. Tostudy the ruggedness of the prepared mixture was observedsix times as a test sample. Small differences in theabsorbance and good consistency were observed afterthree days. An RSD of less than 0.06 % were obtained. Thecomparable absorbance on different days indicates that themethod is capable of producing results with high precision on
 
different days.
 
Thus, the developed method is simple, accurate and preciseand can be used for the routine analysis of Venlafaxinehydrochloride.
Venlafaxine HydrochlorideS.No. Day Wt. of Std Drug
(in mg)
Std. Absorbance % RSD
1 10
th
Mar200910
g/ml0.20160.21820.21960.22940.06214
th
Mar200910
g/ml0.22060.23710.23930.24060.03

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