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Abstract :- A simple, accurate, rapid and precise to an analyst the required data for a given analytical
isocratic reversed-phase high-performance liquid problem, sensitivity, accuracy, range of analysis, precision
chromatographic method has been developed and i.e. the minimum requirements which essentially are the
validated for simultaneous determination of Gabapentin, specifications of the method for the intended purpose to be
Hesperidine and Fosphenytoin sodium in tablet. The able to analyse the desired analyte in different matrices with
chromatographic separation was carried out on an surety and certainty. [3] Using multicomponent analysis
waters C18 analytical column (1504.6 mm; 5 m) with (MCA), a technique that provides accurate quantitation and
a mixture of water:acetonitrile pH 7.0 adjusted with o- identification of unknown components based on known
phosphoric acid (80:20, v/v) as mobile phase; at a flow reference spectra, Multicomponent Analysis is a very
rate of 1 ml/min. UV detection was performed at 214 nm. powerful technique which provides accurate quantitative
The retention times were 5.2, 7.9 and 16.9 min. for results from partially resolved peaks. The MCA process is
Gabapentin, Hesperidine and Fosphenytoin sodium, fast and more accurate than conventional single channel
respectively. Calibration plots were linear (r2>0.999) integration techniques. In addition the purity assessment
over the concentration range 60-180 g/ml for all three feature of MCA provides greater confirmation of peak
drugs. The method was validated for accuracy, precision, identity and homogeneity than many other diode array purity
specificity, linearity, and sensitivity. Validation studies evaluation techniques. [4]
revealed that method is specific, rapid, reliable, and The accuracy in spectral measurements, spectral pattern and
reproducible. The high recovery and low relative the nature of the individual components are key factors for
standard deviation confirm the suitability of the method obtaining reliable results in the simultaneous
for routine determination of Gabapentin, Hesperidine spectrophotometric analysis of multi component mixtures.
and Fosphenytoin sodium in bulk drug and tablet dosage Another important factor contributing towards the precision
form. of analysis of a mixture is relative composition of the
individual components. Nevertheless, a higher absorbance in
Key words: Gabapentin, Hesperidine and Fosphenytoin the case of a minor component will improve the precision.
sodium, RP-HPLC, Anti convulsant, ternary mixture (TM) The selection of wavelengths in a ternary mixture may pose
a little difficulty but it is always preferable to select such
I. INTRODUCTION wavelengths which may fall at a maximum and where there
is least slope of the other two compounds. [5] For each
Analytical methods development and validation play compound in ternary mixture, without searching for the
important roles in the discovery, development, and critical point for the separated peaks, the maximum
manufacture of pharmaceuticals. Pharmaceutical products amplitude of the separated peaks can be measured, it can be
formulated with more than one drug, typically referred to as considered as an advantage of the new method over
combination products, are intended to meet previously alternative methods for the resolution of ternary mixtures.
unmet patients need by combining the therapeutic effects of [6]
two or more drugs in one product.[1] These combination The Fosphenytoin sodium it is chemically known as 5,5-
products can present daunting challenges to the analytical diphenyl-3-[(phosphonooxy) methyl] -2,4-imidazolidinedion
chemist responsible for the development and validation of disodium salt. This is act as anticonvulsant. Structure is
analytical methods. There is a scope, therefore to develop shown in FIG NO.1 [7,8] .The Gabapentin chemically
newer analytical methods for such drugs. Also quality is known as 1-(aminomethyl) cyclohexaneacetic acid also act
important in every product or service but it is vital in as an anticonvulsant. Structure of Gabapentin is shown in
medicines as it involves life. [2] FIG NO.2 [8,9] and the herbal drug Hesperidine chemically
Analytical method development and validation is playing an know as (23)-5-hydroxy-2-(3-hydroxy-4 methoxy phenyl) 7
important role in most of the pharmaceutical industries. The [(2S,3R,4S,5S,6R)-3,4,5 trihydroxy-6-{[(2R,3R,4R,5R,6S)-
method validation should be very useful for industries when 3,4,5-trihydroxy 6 methyloxan -yl]oxymethyl] oxan-2-
introduction of new methods for their routine work. For yl}oxy-2,3-dihydrochromen-4-one. This is act as antioxidant
reporting of new toxicities and patient resistance method and anticonvulsant also. The structure of Hesperidine shown
development and validation should be very important in FIG NO.3 [8,10]
criteria in pharmacy field. Analytical methodology provides
Thus, the aim of the present study is to develop a sensitive Preparation of Standard solution
analytical method for the simultaneous estimation of three
anticonvulsant drugs by Ternary Mixture analysis method Weigh 12 mg Fosphenytoin sodium, 12 mg Gabapentin and
along with their validation by RP-HPLC Method. 12 mg Hesperidine Transfer it into 10 ml volumetric flask,
add 5 ml of methanol. Sonicate it to dissolve and make up
II. MATERIAL AND METHOD the volume with methanol. Pipette out 1 ml from above
solution and transfer in to 10 ml and make the volume with
A. Chemicals And Drugs water.
B. Selection of Mobile Phase (80:20) %v/v was selected, since it gave sharp peaks with
symmetry within limits and significant retention time.
From the various mobile phase tried, mobile phase
containing Orthophosphoric acid in Water: Acetonitrile
Temperature Ambient
Diluent Methanol,Water
GABAPENTIN
100
PEAK AREA (mAU)
80 y = 0.4898x - 7.9512
60 R = 0.9995
40
20
0
0 50 100 150 200
CONCENTRATION (g/ml)
HESPERIDINE
4000
y = 19.826x - 222.2
PEAK AREA (mAU)
3000 R = 0.9998
2000
1000
0
0 50 100 150 200
CONCENTRATION (g/ml)
FOSPHENYTOIN SODIUM
2500
y = 13.297x - 145.57
PEAK AREA(mAU)
2000 R = 0.9994
1500
1000
500
0
0 50 100 150 200
CONCENTRATION (g/ml)
F. Accuracy
Table No.: 4. Result of accuracy study
G. Precision
TM level % Intraday
%RSD
at 9.00 AM at 2.00 PM
Gab Hes Fos Gab Hes Fos
50 0.003 0.009 0.004 0.001 0.001 0.004
H. Specificity
I. Robustness
The proposed method was applied successfully for the mecobalamine in bulk and its tablets world journal of
analysis of GAB, HES and FOS in tablet dosage forms, pharmacy and pharmaceutical sciences .3(12): (2014).
satisfactory results were obtained. [10]. shrikant RK., Anil WK. Analytical method
development for chiral separations of fruity flavonoids
V. CONCLUSION using rp-hplc with improved selectivity and sensitivity.
1(2): 106-113(2010)
The developed RP-HPLC method for the simultaneous
estimation ternary mixture was accurate, precise, linear and
reproducible. This makes the methods suitable for routine
analysis of the combination product in quality control
laboratories.
References