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Pharmaceutical Analysis Articles
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.
METHOD DEVELOPMENT AND VALIDATION OF METRONIDAZOLE IN SOLID DOSAGE FORM BY UV-SPECTROPHOTOMETRIC METHOD
Shahin*,Vemavarapu Satish kumar1
*Shadan Women’s College of Pharmacy. khairtabad, Hyderabad. A.P
1IPQC team member at GRANULES INDIA LIMITED, M.Pharmacy (pharmaceutics) Deevena College of Pharmacy.
A drug may be defined as a substance meant for diagnosis, cure, mitigation, prevention or treatment of diseases in human beings or animals or for alternating any structure or function of the body of human being or animals. Pharmaceutical chemistry is a science that makes use of general laws of chemistry to study drugs i.e. their preparation, chemical nature, composition, structure, influence on an organism and studies the physical and chemical properties of drugs, the methods of quality control and the conditions of their storage etc. The family of drugs may be broadly classified as.
1. Pharmacodynamic agents.
2. Chemotherapeutic agents.
DEVELOPMENT AND VALIDATION OF FIRST ORDER DERIVATIVE METHOD FOR SIMULTANEOUS ESTIMATION OF CEFIXIME TRIHYDRATE AND LINEZOLID IN ITS COMBINED TABLET DOSAGE FORM
Chetana Ribadiya*1, Hemang Ribadia2, Nimish Talaviya3, Chandani Joshi3, Ashok Parmar3
1M.Pharm, Smt. R. B. Patel Mahila Pharmacy College, Atkot
2M.Pharm, Drug Regulatory Affairs Department of Pharmaceutical Science, Saurashtra University
3M.Pharm, Smt. R. D. Gardi B. Pharmacy College, Rajkot
A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Cefixime Trihydrate (CEF) and Linezolid (LNZ) by employing first order derivative zero crossing method in Methanol. The first order derivative absorption at 290 nm (zero cross point of CEF) was used for quantification of Linezolid and 228 nm (zero cross point of LNZ) for quantification of Cefixime Trihydrate. The linearity was established over the concentration range of 2-18 µg/ml and 7-15 µg/ml for Cefixime and Linezolid with correlation coefficient r2 0.9970 and 0.9982, respectively. The mean % recoveries were found to be in the range of 98.36 % – 99.45 % and 100.10 % – 101.66 % for Cefixime and Linezolid, respectively. The proposed method has been validated as per ICH guideline and successfully applied to the estimation of Cefixime and Linezolid in bulk and in market formulation.
DEVELOPMENT AND VALIDATION OF ANALYTICAL METHODS FOR THE SIMULTANEOUS ESTIMATION OF SITAGLIPTIN PHOSPHATE AND METFORMIN HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM
R.B.Desireddy, *Sure.Lakshmi Sindhuri, A. Charitha, G.Naga sowjanya
Nalanda institute of pharmaceutical sciences,
The scope and need of the present work is to develop and validate an analytical method for the analysis of an anti-diabetic drug. Literature survey reveals various UV, HPLC and LC/MS methods are available for individual estimation of the Metformin Hydrochloride and Sitagliptin Phosphate and in combination with other drugs. But, none of the reported analytical methods describe a stability indicating RP-HPLC method for the simultaneous analysis of Metformin and Sitagliptin in tablet dosage form. Hence the present works aims at developing a simple, sensitive, precise, economic and validated second order derivative UV spectroscopic method & stability indicating RP-HPLC method for the simultaneous estimation of Sitagliptin and Metformin in pharmaceutical dosage form. Incomparision with direct UV method, the second order derivative UV spectroscopic method eliminates the interference from UV-absorbing excipients. This method was found to be fast and can be used for formulation screening. HPLC is an integral analytical tool in assessing drug product stability. HPLC methods should be able to separate, detect and quantify the various drug-related degradants that can form on storage or manufacturing, plus detect and quantify any drug-related impurities that may be introduced during synthesis. Stability studies were carried out under various stress conditions like acid hydrolysis, base hydrolysis, water hydrolysis, oxidation, photolytic degradation and under UV-light. Both the drugs Sitagliptin and metformin were degraded more in the alkaline condition.
DEVELOPMENT AND METHOD VALIDATION OF BACLOFEN BY RP-HPLC IN BULK DRUG AND PHARMACEUTICAL FORMULATION
*Kamaldeep singh, Gurvinder Pal Singh, Sandeep Kumar Sharma
Adesh Polytechnic College,
Sri Muktsar Sahib 152026 (Punjab)
In the present work simple and sensitive RP-HPLC method has been developed for the quantitative estimation of Baclofen in bulk drug and pharmaceutical formulations.
A rapid and sensitive RP-HPLC Method with UV detection (253 nm) for routine analysis of Baclofen in Bulk drug and Pharmaceutical formulation was developed. Chromatography was performed with mobile phase containing a mixture of Methanol: Water: Acetic Acid (100:100:0.5) withflow rate 1.0 ml/min The linearity was found to be in the range of 10-50 µg/ml with (r2=0.999) A known amount of the drug solution (80, 100 and 120 %) was added to the powder sample of the tablet formulation and subjected to the estimation of the drug for the recovery studies. There was a high recovery of Baclofen (100.03%, 100.18%, and 100.05%) Robustness of the proposed method was determined by analysis of sample by changes in different parameter like flow rate, detection and Column temperature using similar operational and environmental conditions, the tailing factor was found to be less than 2. The precision of the assay was determined in terms of intra and inter-day variation in the peak area for a set of drug solution (30 µg/ml) assayed three times on the same day and on three different days The intra and inter day variation in the peak ratio of the drug solution was calculated in terms of co-efficient of variation (CV) and obtained by multiplying the ratio of standard deviation to the mean with 100(CV=SD/MEAN X 100)All the parameters are compared with standard raw material of baclofen. The proposed method was validated in accordance with ICH parameters and applied for analysis of the same in marketed formulations.The proposed method was validated by determining sensitivity, accuracy, precision, robustness stability
Mr. Diptesh A. Patel1*, Mrs. Pinkal H. Patel1, Mr. Rohit K. Patel2
1Department of Quality Assurance, Baroda college of pharmacy, Vadodara, Gujarat, India.
2Department of Quality Assurance, Kaptab Pharmaceutical, Vadodara, Gujarat, India.
The purpose of the research investigation was to study concurrent Process Validation of Cefixime Dispersible TabletI.P. These processes should be controlled in order that the finished product meets all quality specifications. The critical process parameters were identified with the help of process capability and evaluated by challenging its lower and upper release specifications. Three initial process validation batches of same size, method, equipment and validation criteria were taken. The critical parameter involved in sifting, sizing and compression stages were identified and evaluated as per validation plan. Uniformity of mixing is optimum in 30 min as standard deviation was between ±0.20% to ±0.99%. Compression speed of 16 RPM was suitable for IPQC as % standard deviation limits was found for Thickness was ±1.8 % to ±3 %, Hardness ±16.6 % to ±37 %, Weight Variation ±0.3% to ±7.1 %, Friability ±2.4 to ±7.1 %, Diameter ±0.9 % to ±1.2 % and Disintegration time NMT 3 min. The outcome indicated that this process validation data provides high degree of assurance.
DEVELOPMENT AND VALIDATION OF BIOANALYTICAL METHOD FOR SIMULTANEOUS ESTIMATION OF ETAMSYLATE AND MEFENAMIC ACID IN HUMAN PLASMA BY RP-HPLC METHOD
Mona Karia*1, Bhargav Gohel2, Bina Thanki3, Darshan Madiya4, Shital Faldu5
1,3M.Pharm, Smt. R.D.Gardi B.Pharmacy College. Rajkot, Gujarat, India
2Q.A. Officer, Intas Pharmaceutical Ltd., Ahemdabad.
4Assistant Professor of Smt. R.D.Gardi B.Pharmacy College, Rajkot
5Principal of Smt. R.D.Gardi B.Pharmacy College, Rajkot
An accurate, simple, precise and sensitive HPLC method with UV detection was developed and validated for simultaneous estimation of Etamsylate and Mefenamic acid in human plasma as per USFDA guidelines. Etamsylate and Mefenamic acid were spiked with human plasma and 5 % w/v Trichloro acetic acid used for protein precipitation in ration of 1:9 %v/v of human plasma. The column used was SUSEIDO C18 column (250mm x 25 mm, i.d, 5 µ). Analysis was carried out with Methanol: ACN (70:30 % v/v): Buffer (0.05M Ammonium acetate buffer) pH 6.0 (85:15,% v/v) as mobile phase at flow rate of 1.5 ml/min at 298 nm with UV detection. The retention time of Mefenamic acid observed was 1.98 min and for Etamsylate 3.85 min respectively. The method was validated over the range of 0.5-30 μg/ml for Etamsylate and 0.2-18 µg/ml for Mefenamic acid with coefficients of regression 0.9939 and 0.9914 for Etamsylate and Mefenamic acid respectively. LOD and LOQ were 0.17 ng/ml and 0.51 ng/ml for Etamsylate and 2.62 ng/ml and 7.95 ng/ml for Mefenamic acid.The mean % recovery for MEF and ETM were found to be 89.07% and 88.98%with % C.V. of 1.87% and 1.91% respectively. Inter-day as well intra-day replicate, gave % RSD below 4.44 and 2.63 for Etamsylate and 3.20 and 3.75 for Mefenamic acid respectively. This RP-HPLC method is sensitive, selective, accurate, precise and rapid for the simultaneous estimation of Etamsylate and Mefenamic acid in human plasma with limit of Quantification in nano-gram level was developed and validated as per USFDA guideline and can be applied for a bioequivalence study to compare relative bioavailability of drug.