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Pharmaceutical Analysis Articles
NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION OF LOSARTAN POTASSIUM AND AMLODIPINE DRUGS IN PURE AND PHARMACEUTICAL DOSAGE FORMS
1Kumari Jyothsna*, 2N.Chandana
1,2Department of Pharmaceutical Analysis and Quality Assurance,
Nimra College of Pharmacy, Jupudi, Vijayawada, A.P, India
A fast, robust and accurate RP-HPLC method was developed and validated for simultaneous determination of Losartan potassium and Amlodipine in tablets. The mobile phase was mixture of aqueous Tri ethyl amine with pH 2.0 and Acetonitrile(70:30), effluent flow rate monitored at 1.0 ml/min. the stationary phase was C18 column, 3µm(4.6×250mm). The solutions of standard and the sample were prepared in methanol. The retention times was found to be 2.916min and 5.214min for Losartan potassium and Amlodipine respectively at 246nm. Calibration graphs constructed at their wavelengths of determination were linear in the concentration range of 50-150µg/ml. The percentage assay for Losartan potassium and Amlodipine were found to be 101% and 100%respectively. The method was validated and it was found to be accurate, precise, linear and reproducible as per ICH guidelines.
A NOVEL RP- HPLC METHOD DEVELOPMENT AND VALIDATION OF ATORVASTATIN AND FENOFIBRATE IN BULK AND PHARMACEUTICAL DOSAGE FORMS
1Vinjam Swathi* 2Nanda Kishore Agarwal
1M pharmacy, Department of Pharmaceutical Analysis and Quality Assurance, Nimra College of Pharmacy, Jupudi, Vijayawada, A.P, India
2Professor and head of the department of pharmaceutical chemistry, Nimra College Of Pharmacy, Jupudi, Ibrahimpatnam, Vijayawada, A.P, India
The present investigation describes about a simple, economic, selective, accurate, precise reverse phase high performance liquid chromatographic method for the simultaneous estimation of Atorvastatin and Fenofibrate in pure and pharmaceutical dosage forms. Atorvastatin and Fenofibrate were well separated using a Thermohypersil BDS C18column of dimension 100 × 4.6, 5µm and Mobile phase consisting of Methanol: Water (Adjusted with orthophosphoric acid to pH-2) in the ratio of 40:60v/v at the flow rate 1 ml/min and the detection was carried out at 274nm with PDA detector. The Retention time for Atorvastatin and Fenofibrate were found to be 1.438, 2.949 respectively. The developed method was validated for recovery, specificity, precision, accuracy, linearity according to ICH guidelines. The method was successfully applied to Atorvastatin and Fenofibrate combination pharmaceutical dosage form.
Satya Lakshmi.B*, P.Raju vel, Dr. P. Venkateswara Rao, Sindhu.G, Nikil Kumar.K
A.M Reddy Memorial College of Pharmacy,
Narasaraopet, AN University, Guntur.
The reliability of quantitative assays in determination of drugs in biological fluids using High-performance liquid chromatography with Tandem Mass spectrometric determination (LC-MS/MS) detection methods and the integrity of resulting Pharmacokinetic data may not be absolute, in contrary to common perceptions and possible conjectures. The results may be adversely affected by lack of specificity and selectivity due to ion suppression caused by the sample matrix and interferences from metabolites. The advancements in the past few years and new technologies introduced can be used in enhancing LC-MS/MS Bio-analytical method development by reducing matrix effects. This Article reviews Automated Sample preparation and various extraction techniques like liquid-liquid extraction, Solid phase extraction and protein precipitation which plays an important role in sample preparation and detection by LC-MS/MS. Potential drawbacks during method development and validation are pointed out.
Narsinh N. Potdar*, Pranita P. Kore, Rishikesh V. Antre
Department of Pharmaceutical Chemistry,
JSPM’s Charak College of Pharmacy and Research, Wagholi,
Pune-Nagar Road, Pune-412 207 (India)
Three new simple, economic spectrophotometric methods were developed for quantitative estimation of Rosuvastatin Calcium in bulk formulation. First method includes determination of Rosuvastatin Calcium at absorption maxima 252 nm, second method applied was area under curve for analysis of Rosuvastatin Calcium in the wavelength range of 247-257 nm and third method was first order derivative. Beer law obeyed in the concentration range of 5-35 μg/ml for all three methods. The correlation coefficients were found to be 0.974, 0.982 and 0.982by absorption maxima, area under curve and first order derivative spectra. Results of analysis were validated statistically and by performing recovery studies. The mean percent recoveries were found satisfactory for all three methods. The percentage label claim was found in the range of 100.28% to 101.01% .The proposed method was validated statistically and recovery studies.
REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC ESTIMATION OF ATAZANAVIR AND RITONAVIR IN PHARMACEUTICAL DOSAGE FORM
Venkatesh. J , M. Singaiah Chowdary*, Haritha. D, Anuroop , Dr. V.V.L.N Prasad, Anjani Prasad Reddy. V.
Department of Pharmaceutical Analysis and Quality assurance,
School of pharmacy, Anurag Group of Institutions, Venkatapur (V).
Ghatkesar (M), Rangareddy (D)
A new simple, rapid, specific, accurate, precise and novel reverse phase High Performance Liquid Chromatography (RP-HPLC) method has been developed for the simultaneous estimation of atazanavir and ritonavir in the combined pharmaceutical dosage form. The chromatographic separation for Atazanavir and Ritonavir were achieved with mobile phase containing mixed phosphate buffer (pH 4.0) and acetonitrile (45:55 % v/v), Symmetry C18 (4.6 x 100mm, 3.5mm, Make: ACE)at 5°C and UV detection at 237 nm. The compounds were eluted in the isocratic mode at a flow rate of 0.9 ml min-1. The retention times of atazavir 4.29 ± 0.09 min and ritonavir at 5018 ± 0.09 min. The above method was validated in terms of linearity, accuracy, precision, LOD, LOQ etc. in accordance with ICH guidelines.
B. Madhavi*, Dr. P.Venkateswara Rao, P.Rama Bharathi, T.Swathi, BH. Ramya Reddy
A.M Reddy Memorial College of Pharmacy, Narasaraopet
ANU University, Guntur.
The aim of the present work was focused on development of analytical methods for the estimation of drugs in multi component dosage form. There is a plethora of analysis of such formulations without prior separation. For the estimation of multi component formulation, the instrumental techniques, which are commonly employed, are spectrophotometry, Gas liquid chromatography (GLC), high performance thin layer chromatography (HPTLC), high performance liquid chromatography (HPLC) etc. These methods are based upon the measurement of specific and non specific physical properties of the substances. Chromatographic separation techniques are one of the most widely used technique for analysis of a multi component formulation. HPLC techniques allows for the separation as well as analysis of different drugs that are present in a combined formulation. Validation studies were performed in order to assess the validation parameters for the analytical method developed in accordance to ICH Guidelines.
Mr. Vivek P. Chavda, Dr. Moinuddin M. Soniwala
Department of Pharmaceutics, B.K. Mody Government Pharmacy College,
Rajkot – 360003, Gujarat (India)
In recent years, many important initiatives have been undertaken by regulatory authorities and industry associations to promote international harmonization of regulatory requirements. International Conference on the Harmonization of Technical Requirements for the Registration of Pharmaceuticals for Human Use (ICH) was organized in April 1990 and has as its sole and primary purpose the creation of international standards for the purpose of pharmaceutical research. This process was initiated in order to harmonize the submission requirements for new pharmaceuticals in the three main regions of Europe, the United States, and Japan and to avoid duplication, inefficiencies and delays.
The six cosponsors of ICH were
- European Commission,
- European Federation of Pharmaceutical Industry Association (EFPIA),
- Japanese Ministry of Health (MHW),
- Japanese Pharmaceutical Manufacturers Association (JPMA),
- Food and Drug Association (FDA), and the Pharmaceutical Research
- Manufacturers of America (PhRMA)
DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF PARACETAMOL AND PAMABROM IN BULK DRUG AND IN ITS SYNTHETIC MIXTURE
Nimish Talaviya1*, Nirav Chandegara2, Rakesh Radadiya3, Chetana Ribadiya4, Chandani Joshi5, Dhara Kanjaria6
1,5Department of Q.A., Smt. R. D. Gardi B. Pharmacy College, Rajkot
2Department of Pharmacology, K. B. Institute of Technology, Gandhinagar
3Department of Q.A., Mts. V.B. Manvar College of Pharmacy, Dumiyani
4Department of Q.A., Smt. R. B. Patel Mahila Pharmacy College, Atkot
6Department of Q.A., Shree H. N. Shukla Institute of Pharmaceutical Education & Research, Rajkot
This paper presents a RP-HPLC method for the simultaneous estimation of Paracetamol and Pamabrom in its synthetic mixture. The process was carried out on C18 (250 x 4.6mm, 5µ) (Spincotech Pvt. Ltd.) column using Phosphate buffer pH 4.5: Acetonitrile (75:25 %v/v) where pH was maintained using 0.1% orthophosphoric acid as a mobile phase at a flow rate of 0.8ml/min. Detection wavelength was fixed at isobestic point 268 nm. Linearity was observed in the concentration range of 10-50 μg/ml for Paracetamol (r2=0.9986) and 15-75 μg/ml for Pamabrom (r2=0.9971). The retention time of Paracetamol and Pamabrom was found to be 2.665 and 6.907 minutes respectively with resolution 13.70. The developed method is simple, precise, specific, robust, rapid, reproducible, and sensitive and it can be used for estimation ofParacetamol and Pamabrom in its synthetic mixture.
DEVELOPMENT AND VALIDATION OF LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRIC METHOD FOR THE QUANTIFICATION OF CIPROFIBRATE FROM HUMAN PLASMA
Emanual Michael Patelia*, Rakesh Thakur, Jayesh Patel
Department of Pharmaceutical analysis and chemistry (Gujarat technical university)
Department of Pharmacology (University of Bedfordshire)
To develop and validate liquid chromatography-tandem mass spectrometric method for the quantification of ciprofibrate from human plasma. Ciprofibrate and furosemide (IS) were extracted from human plasma using Oasis HLB 1cc 30 mg solid phase extraction cartridge. The chromatographic separation was performed on ACE C18, 50×4.6 mm, 5μ column. The mobile phase consisted of 0.001% ammonia in methanol-acetonitrile-water (70:20:10, v/v/v) was delivered at rate of 1 mL/min. Detection and quantitation were performed by a triple quadrupole equipped with electrospray ionization and multiple reaction monitoring in negative ionization mode (API 3200). The most intense [M-H]- transition for ciprofibrate at m/z 287.0→85.0 and for IS at m/z 328.9.0→204.9 were used for quantification. The developed method was successfully applied for bioequivalence study of ciprofibrate. The method was found to linear over the range of 25-30000 ng/mL (r>0.998). The lower limit of quantitation (LLOQ) was 25 ng/mL. The extraction recovery was above 90%. The accuracy was found to 101.26%-106.44%. The intra and inter-day precision expressed as % CV were 1.15% and 5.25%, respectively. The stability testing was also investigated and it was found that both drug and IS were quite stable. A simple, rapid, sensitive, accurate and precise LC-ESI/MS/MS method has been developed for the quantification of ciprofibrate from human plasma using SPE method. The method exhibited good linear response over the selected concentration range 25-30000 ng/mL. Selectivity and sensitivity were sufficient for detecting and quantifying ciprofibrate in human plasma. These features coupled with a short run time at 1.8 min compared to reported methods, facilitated a high analysis throughput, with the ability to quantify a larger number of clinical samples in a shorter time frame.
ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ZINC PYRITHIONE IN KETOCONAZOLE SHAMPOO BY RP-HPLC METHOD
Sahoo.U1*, Sethy.S.P1, Biswal.S1, Patro.S.K1, Banerjee.M1, Sundeep Kumar.H.K.S1, Patel.D2
*1Department of Pharmaceutical Chemistry
Institute of Pharmacy and Technology, Salipur, Cuttack, Odisha-754202
2ZYG Pharma, Pvt, Ltd, Pithampur, Madhya Pradesh
A mobile phase consisting of Acetonitrile and water in the ratio of 60:40 gave a well resolved and sharp peak for Zinc-Pyrithione with a retention time of 11.61 mins. The flow rate was 1 ml/min and effluent was monitored at 322 nm. Zobrax C18 column, run time of 30 min and ambient temperatures were found to be optimum for the analysis. System suitability was performed by injecting five replicate injections of working standard solution. The System suitability results obey all the parameters and found within the acceptable range. The precision study was found to be less than 1 (% RSD). So, it indicates the method is precise. The recovery study was found to be 98 to 102 % and % RSD was found to be less than % 1. So, the method is more accurate, precise, and sensitive.