Shri Prakashchand Jain College Of Pharmacy & Research,Palaskhede
A new, simple, accurate , rapid and precise spectrophotometric method has been developed for validation of Gemfibrozil (GEM) in bulk drug. An attempt was made to preclude the use of corrosive inorganic solvents by the use of 1 M NaOH. The developed method was the measurement of absorptivity at 274nm . The results of analysis have been validated as per ICH guidelines. The Concentrations of this drug were evaluated in laboratory mixture and marketed formulation. Accuracy was determined by recovery studies from marketed formulation and Ranges From 99.63 – 100.93%. Precision of method was find out as repeatability shows the values within acceptable limit.
Gemfibrzil (GEM) is a dimethylphenoxy derivative 5-(2,5- dimethylphenoxy)-2,2-dimethylpentanoic acid.(fig.-1) . It is a lipid regurating agent used in the treatment of hyperlipidemia. similar to clofibrate, is used to treat hyperlipoproteinemia and as a second-line therapy for type IIb hypercholesterolemia. Gemfibrozil increases the activity of extrahepatic lipoprotein lipase (LL), thereby increasing lipoprotein triglyceride lipolysis. It does so by activating Peroxisome proliferator-activated receptor-alpha (PPAR?) 'transcription factor ligand', a receptor that is involved in metabolism of carbohydrates and fats, as well as adipose tissue differentiation. Chylomicrons are degraded, VLDLs are converted to LDLs, and LDLs are converted to HDL. This is accompanied by a slight increase in secretion of lipids into the bile and ultimately the intestine. Gemfibrozil also inhibits the synthesis and increases the clearance of apolipoprotein B, a carrier molecule for VLDL. Well absorbed from gastrointestinal tract (within 1-2 hours). Gemfibrozil mainly undergoes oxidation of a ring methyl group to successively form a hydroxymethyl and a carboxyl metabolite. Approximately seventy percent of the administered human dose is excreted in the urine, mostly as the glucuronide conjugate, with less than 2% excreted as unchanged Gemfibrozil. Half life of the drug was 1.5 hrs and more than
95% of the drug was bound to plasma.
Fig-1. Structure of Gemfibrozil
Chemical name: 5-(2, 5-dimethylphenoxy)-2, 2-dimethylpentanoic acid
Chemical formula:
EXPERIMENTAL :
Instrumentation :
UV experimentation was performed on Shimadzu 1800 UV-visible spectrophotometer equipped with Photo Diode Array (PDA) detector, with 1 cm quartz cell. Citizen Digital Ultrasonic Cleaner was used for solubility purpose.
MATERIALS AND METHODS :
All reagents used are AR grade and gemfibrozil was gift sample obtained from flamingo Laboratories, mumbai and were used as reference standard. The tablet formulation was purchased from local market.
Preliminary solubility study :
Solubility of drug was determined at 27 ±1°C. Gemfibrozil (10mg) was added in 10 ml volumetric flask and 10ml 0f 1M NaOH was added in it. The clear solution of Gemfibrozil was obtained.
Preparation of standard stock solutions:
Gemfibrozil standard stock solution: (1000µg/ml).An accurately weighed Gemfibrozil (10mg) was added in 10 ml volumetric flask and dissolved in 1M NaOH and volume was made up to the mark using 1M NaOH to get final concentration(1000µg/ml).
Study of spectra and selection of wavelength:
The aliquot portions of standard stock solutions of Gemfibrozil were diluted appropriately with 1M NaOH to obtain concentration 10 ?g/mL of drug. The solutions shown in Fig. 2. From the spectrum wavelength selected for estimation of drug was 274.nm as ? max of Gemfibrozil.
Fig.2 Spectrum Of Gemfibrozil At The Wavelength 274
STUDY OF LINEARITY CURVES :
The aliquot portions of standard stock solutions of Gemfibrozil was diluted appropriately with 1M NaOH to get a series of concentration from 10-50µg/mL for drug. The absorbance of this drug was measured at 274nm respectively and calibration curve was plotted as concentration versus absorbance
Linearity and Range :
The suitable aliquots was taken to obtain 10, 20, 30, 40, 50 µg/ml. from GEMFIBROZIL (1000µg/ml) stock solution. The results are shown in fig. no. 3,
Fig 3-linearity curve of Gemfibrozil
Gemfibrozil obeyed linearity in the concentration range of 10-50 ?g/ml respectively at ? max 274 nm with correlation coefficient (r2 > 0.99) in this case. Marketed brand of tablet was analyzed.
Analysis of Marketed Formulation by Proposed Method:
20 capsule was accurately weighed, and reduced to fine powder. An accurately weighed powder sample equivalent to 10 mg of gemfibrozil was transferred to 10 ml volumetric flask and 1M NaOH was added in it. Sonicate it for 20 min. The solution was filtered through Whatmann filter paper no. 41. The filtrate was further diluted with 1M NaOH to get final concentration (1000µg/ml). From this solution 10µg/ml was prepared. The absorbance of sample solution was measured at 274 nm and the result is shown in Table No. 1.
Table No. 1: Results of Application of Proposed Method for Analysis of Marketed Formulation
VALIDATION METHOD
Accuracy
Accuracy of each of the proposed method was ascertained on the basis of recovery studies performed by standard addition method as shown in the table no.2.
Table no.2 Accuracy study -
*mean of each 3 reading
Precision
Precision of the analytical method is expressed as the series of the measurement. It was ascertained by replicate estimation of the drug by the proposed method as shown in table no.3.
Table no.3 Precision-
*mean of each 3 reading
Repeatability:
Repeatability was ascertained by getting the sample analyzed by different analyst and carrying out analysis for no. of times. The results are shown in table no. 04
Table no.4 Repeatability study-
Label Claim:
RESULT AND DISCUSSION :
The method was optimized with view to develop a rapid, simple, accurate method for validation of Gemfibrozil in bulk & pharmaceutical formulation. uv scanning at 400-200nm of Gemfibrozil shows that 274 nm is the suitable wavelength for detection of drug.(fig.2).Gemfibrozil shows linearity in the concentration range of 10-50µg/ml (r2-0.993) respectively .recovery study of drug were carried out for the accuracy parameter this study where carried out at three levels( 80%, 100%, 120% ) by standard addition method. The mean recovery was found to be 99.41% for Gemfibrozil respectively. The developed method was found to be simple, precise, specific, & accurate Therefore this method can be applied for routine analysis of drugs in formulation & in bulk drug.
CONCLUSION :
The developed method is suitable for validation of Gemfibrozil in pharmaceutical dosage form is accurate, precise, robust and rapid. Therefore this method can be applied for routine analysis of drugs in formulation & bulk drug.
ACKNOWLEDGEMENT :
The authors are thankful to Flamingo Laboratories, Mumbai for providing gift samples of Gemfibrozil respectively.
REFERENCES
Books and Textbooks
Journals and Articles
Specific Articles and Papers
Regulatory Guidelines
Online Databases
Research Institutions and Organizations
Books and Textbooks
Journals and Articles
Specific Articles and Papers
Regulatory Guidelines
Online Databases
Research Institutions and Organizations
Pallavi Patil , Premjit Pawar, Rutuja Narwade, Kajal Patil, Harshada Patil, Janvhi Patil , Development And Validation Of A UV Spectrophotometry Method For Gemfibrozil In Bulk And Pharmaceutical Dosage Forms, Int. J. of Pharm. Sci., 2024, Vol 2, Issue 9, 518-523. https://doi.org/10.5281/zenodo.13737731
10.5281/zenodo.13737731
