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05/02/2023 1
PRESENTED BY MR.VILAS H.KAMBLE
GIUDED BY DR.MRS SONALI MAHAPARALE
DR.D.Y.PATIL COLLEGE OF PHARMACY AKURDI,PUNE.
DEVLOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS
ESTIMATION OF MUSCLE RELAXANT AND ANALGESIC DRUG IN PURE AND
PHARMACEUTICAL DOSAGE FORM
05/02/2023 2
CONTENT Literature survey Principle Need of work Aim and objective Plan of work Drug profile Experiment Outcome of study expected References
05/02/2023 3
LITRATURE SURVEY 1 2
JOURNAL NAME
International journal of pharmacy and pharmaceutical science
International journal of pharmacy and
pharmaceutical science
AOUTHER NAME
Nimila Carolin,Balan P. et. al. Patel Madhavi Bhawani Singh et. al.
METHOD NAME RP HPLC of Tolperisone and Paracetamol
UPLC of Tolperisone and Paracetamol
COLUMN NAME Symmetry C18 250×4.6mm UPLC BEH C18 50mm×2.1mm
MOBILE PHASE Water:ACN (60:40) Water:ACN (30:70)
WAVELENGTH
258 nm 254 nm
FLOW RATE 0.7 per min 0.20ml per min RT Tolperisone=2.25,Paracetamol=3.
29Tolperisone=1.396,Parac
etamol=2.625
05/02/2023 4
LITRATURE SURVEY 3 4
JOURNAL NAME
Pelagia Research LibraryInternational journal of
pharmacy and pharmaceutical science
AOUTHER NAME Satyanarayana M. V Anuradha. V. et al
Thippeswamy M. Somanna P. at al
METHOD NAME RP HPLC of Tolperisone and
Paracetamol RP HPLC of Paracetamol
COLUMN NAME Hypersil BDS, 150 x
4.6mm C18C18 colum (250 mm X 4.6 mm i. d, 5 μm particle size)
MOBILE PHASE Buffer:ACN (70:30) pH 3
with TEAACN;Phospahte Buffer(15:85)
WAVELENGTH
267 nm. 210 nm
FLOW RATE1.0 Per Min 1.0 ml/min
RT Tolperisone=4.6,Paracetamol=2.3
5.7 minutes
05/02/2023 5
CHROMATOGRAPHYPrinciple- When a mixture of components are introduced
into a HPLC column, they travel according to their relative affinities towards the stationary phase.
The component which has more affinity towards stationary phase travel slower.
The component which has less affinity towards stationary phase travel faster.
Since no two component have the same affinity towards the stationary phase, the component are separated.
05/02/2023 6
CHROMATOGRAPHY
FIG.SEPARATION OF COMPONENT BY HPLC
05/02/2023 7
NEED OF WORK Simultaneous estimation of muscle relaxant
and analgesic drug combinationReduce time of analysis Increase accuracy of analysis Reduce cost of analysis
05/02/2023 8
AIM AND OBJECTIVE To develop method for simultaneous
estimation of muscle relaxant and analgesic drug by using RP-HPLC method.
To validate the developed method as per ICH guidelines.
05/02/2023 9
PLAN OF WORK Literature survey
Selection of drug Study of
physicochemical
properties of
drugs
Optimisation of
analytical method Validatio
n of developed method
Force degradation study
Result and
discussion
Summary and
conclusion
05/02/2023 10
DRUG PROFILE SR NO
PARAMETER MASCLE RELAXANT DRUG
ANALGESIC DRUG
1 Chemical Structure
2 Chemical name
2-methyl-1-(4-methyl phenyl)-3-(1-piperidinyl)-1-
propsnone
N-(4-hydroxyphenyl)-acetamine
3 Molecular formula
C16H23NO.HCl C8H12 NO2
4 Category Muscle relaxant Antipyretic analgesic 5 Melting range Litrature-176-177 Litrature-169-170
6 Dissociation constant /pKa
value
9.4 9.5
05/02/2023 11
EXPERIMENT
Solubility study SR NO
SOLVENT /BUFFER SOLUBILITY
MUSCLE RELAXANT DRUG
ANALGESIC DRUG
1 Water Very soluble Sparingly soluble 2 Acetonitrile Very soluble Freely soluble
3 Methanol Very soluble Very soluble 4 Acetone Soluble Freely soluble 5 Chloroform Very soluble Practically
insoluble 6 Tetra hydro furan Soluble Soluble 7 Ethyl acetate Very slightly
soluble Soluble
8 Isopropyle alcohol Freely soluble Freely soluble
Solubility in solvent
05/02/2023 12
EXPERIMENT Solubility in buffer
SR NO
NAME OF BUFFER pH SOLUBILITY OF DRUG
MUSCLE RELAXANT DRUG
ANALGESIC DRUG
1 0.1M Ammonium acetate buffer
6.50 Soluble Sparingly soluble
2 0.1M Potassium dihydrogen phosphate buffer
4.75 Freely soluble Sparingly soluble
3 0.1M Sodium dihydrogen phosphate buffer
4.66 Freely soluble Freely soluble
4 0.1M Dipottasium hydrogen phosphate
9.76 Sparingly soluble Soluble
5 0.1 M Disodium hydrogen phosphate
9.82 Sparingly soluble Soluble
05/02/2023 13
EXPERIMENT Melting point determination
SR NO NAME OF DRUG OBSERVED MELTING POINT
1 Muscle Relaxant drug
176.5-177.7
2 Analgesic Drug 170.3-173.5
05/02/2023 14
EXPERIMENT λmax determination By preparing 10 ppm solution of muscle
relaxant drug and analgesic drug individually and scanning in UV at 200nm-400nm
• Preparation of diluents for λmax determination
Selected diluents ratio-70:30
SR NO
DILUENT RATIO(WATER:ACN)
SOLUBILITY OF MUSLE RELAXANT DRUG
SOLUBILITY OF ANALGESIC DRUG
1 90:10 Freely Soluble Very Slightly Soluble
2 80:20 Freely Soluble Soluble 3 70:30 Freely Soluble Freely Soluble
05/02/2023 15
EXPERIMENT Muscle relaxant drug
λmax of Muscle relaxant drug was found to be 260nm
05/02/2023 16
EXPERIMENT Analgesic Drug
λmax of Analgesic Drug was found to be 246nm
05/02/2023 17
EXPERIMENT • pH determination By preparing 10% solution of each drug in
water and observed pH on pH meter
SR NO DRUG CATEGORY
OBSERVED pH Of 10% solution
1 Muscle relaxant drug
4.70
2 Analgesic drug 6.353 Water 6.50
05/02/2023 18
EXPERIMENT Selection of mobile phase• Selected mobile phase-Water:ACN• Ratio-50:50• Chromatographic condition
SR NO
PARAMETER DISCRIBTION
1 Mode Isocratic 2 Column Hypersil BDS,
C18,150×4.6,5Micrion 3 Wavelength 254nm 4 Flow Rate 1ml Per Min 3 Column Oven
Temperature 30 Degree Celsius
4 Injection Volume 20 Micro Litter 5 Run Time 60 Mins
05/02/2023 19
EXPERIMENT Blank
05/02/2023 20
EXPERIMENT Muscle relaxant drug standard
05/02/2023 21
EXPERIMENT Analgesic drug standard
05/02/2023 22
WORK DONE Observation
Sr No
Drug Category
Retention Time
Area Theoretical Plates
Asymmetry
1 Blank 1.60 1725 2844 1.342 Muscle
Relaxant Drug Std
- - - -
3 Analgesic Drug Std
0.95 34933940
784 1.35
05/02/2023 23
OUTCOME OF STUDY EXPECTED
The accurate and precise method for simultaneous estimation of both the drug
Simple methodCost effective method Less time consuming method
05/02/2023 24
REFRENCES Carolin N, Balan P. Development and Validation
of A Reverse Phase HPLC Method of Simultaneous Estimation of Tolperisone Hydrochloride and Paracetamol in tablet dosage form, International Journal of Pharmacy and Pharmaceutical Science,2012,4(5),84-88.
Patel M. Parmar R. The Simultaneous Estimation of Paracetamol and Tolperisone Hydrochloride in Tablet by UV Spectrophotometric Methods, Jouranl of Pharmaceutical Science and Bioscientific Research, 2012, 2(2),63-67.
Chatwal G. Anand S. Instrumental Method of Chemical Analysis, Himalaya Publishing House, 2012, fifth edition, 2.624-2.639
05/02/2023 25
REFRENCES Thippeswamy M. Somanna P. A New Method
Development and Validation for Estimation of Paracetamol In Pharmaceutical dosage form by RP-HPLC, International Journal of Pharmacy and Pharmaceutical Sciences, 2015, 7(8), 190-194.
Beckett A . Stenlake J . Practice Pharmaceutical Chemistry. CBS Publisher, 4th Edition, Part II. New Delhi,285-288.
Sharma K. Patel P. First Derivative Spectrophotometric Method for the Simultaneous Estimation of Tolperisone and Paracetamol in their Combined Dosage Form, Journal of Pharmaceutical Sciences and Bioscientific Research, 2012,2(2),92-96.
05/02/2023 26
REFRENCES Mathew M. Puthusseri S. Validated HPTLC
Method for Simultaneous Estimation of Tolperisone Hydrochloride And Paracetamol In Tablet Dosage Form, World Journal of Pharmaceutical Research, 2012,3(10), 513-522.
Patel M. Singh B. Stability Indicating UPLC Method for Quantification of Tolperisone HCl and Paracetamol from muscle relaxant combination tablet, International Journal of Pharmacy and Pharmaceutical Sciences, 2015,7(8),300-304.
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