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Pharmaceutical Analysis Articles


BIO-ANALYTICAL METHOD DEVELOPMENT, VALIDATION AND TRANSFER BY USING LC-MS/MS – A REVIEW

About Authors:
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.
balla.satya03@gmail.com

Abstract:
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.


SPECTROPHOTOMETRIC DETERMINATION OF ROSUVASTATIN CALCIUM IN MARKETED FORMULATION

About Authors
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)

*narsinh_potdar@rediffmail.com

Abstract
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

ABOUT AUTHORS:
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)
*chowdary.mannam1@gmail.com

ABSTRACT:
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.


METHODS FOR THE ESTIMATION AND VALIDATION OF MULTICOMPONENT FORMULATION

About Authors:
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.
*madhavi.pharm@gmail.com

Abstract:
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.


PHOTOSTABILITY TESTING

ABOUT AUTHOR:
Mr. Vivek P. Chavda, Dr. Moinuddin M. Soniwala
Department of Pharmaceutics, B.K. Mody Government Pharmacy College,
Rajkot – 360003, Gujarat (India)
vivek7chavda@gmail.com

INTRODUCTION1,2
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

  1. European Commission,
  2. European Federation of Pharmaceutical Industry Association (EFPIA),
  3. Japanese Ministry of Health (MHW),
  4. Japanese Pharmaceutical Manufacturers Association (JPMA),
  5. Food and Drug Association (FDA), and the Pharmaceutical Research
  6. 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

About Authors:
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
*nimish.talaviya@gmail.com

Abstract
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

About Authors:
Emanual Michael Patelia*, Rakesh Thakur, Jayesh Patel
Department of Pharmaceutical analysis and chemistry (Gujarat technical university)
Department of Pharmacology (University of Bedfordshire)
ricky.emanual@gmail.com

Abstract:
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

ABOUT AUTHORS:
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
sarada9439504350@gmail.com

ABSTRACT-
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

ABOUT AUTHORS:
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.
*shahins333@gmail.com

INTRODUCTION
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

ABOUT AUTHORS:
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
*chetana.ribadiya@gmail.com

ABSTRACT
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.


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