'Hplc method' diaporamas de présentation

Frederic Forini Waters Corporation European Headquarters April 17-20, 2012

Understanding the Proposed Changes to USP General Chapter <621>. Frederic Forini Waters Corporation European Headquarters April 17-20, 2012 New Munich Trade Fair Centre. What is the USP? . The United States Pharmacopeia (USP) is an independent, official public standards-setting authority

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The role of chromatography in physico-chemical characterisation

The role of chromatography in physico-chemical characterisation. Shenaz Nunhuck CASS, GSK. Why do we need physchem measurements?. Physicochemical properties of drugs influence their absorption and distribution in vivo Systemic absorption of drug involves a number of rate processes:

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Dr. Helmut Krause Global Manager RSTS

Restricted Substances ?????? The Importance of Proper Testing and Proper Testing Procedures ????????? Dongguan, 21 th September 2006. Dr. Helmut Krause Global Manager RSTS. Restricted Substances List (RSL) ????????. Typical Test Parameters of RSL pH Value ??? ??? Formaldehyde ??? ????

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Validation of stability indicating rp-hplc method for the assay of ibrutinib in pharmaceutical dosage

A stability indicating RP-HPLC method was developed and validated as per international chemical harmonization guidelines, and adopted for the assay of Ibrutinib in bulk and tablet dosage forms. The chromatographic separation was carried out by using Waters (Alliance) HPLC 2695 series system equipped with UV-Visible spectrophotometer as detector. Mobile phase composed of 0.1% Orthophosphoric acid buffer and acetonitrile in the ratio 70:30 %v/v was allowed to flow through Inertsil ODS 100mm x 4.6 mm, 5uf06dm column at a flow rate of 0.8ml/minute, maintaining the column temperature at 30u00b0C. About 20u00b5l of standard or sample solution was injected into the column and the components were detected at a wavelength of 320nm. System precision and method precision of the proposed method was evaluated as %RSD and found to be 1.7252 and 1.0583 respectively. Accuracy of the developed method as percent of mean recovery at three different concentrations 50, 100 and 150% with respect to target concentration was determined and found to be 100.68, 100.90 and 100.33 respectively. The peak area was found to be proportional to concentration of Ibrutinib within the linearity limits 3.5-21.0u00b5g/ml, slope, intercept and correlation coefficient were determined by linear regression analysis. The developed method was found to be robust and rugged and was applied for quality control analysis of pharmaceutical formulations. The stability of the drug under different degradation conditions was examined and found to be stable. The proposed method was found to be simple and suggested for an alternative method in quality control in any quality control laboratories.

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Analytical Method Validation of RP-HPLC Method for Simultaneous Estimation of Levonorgestrel

The aim of recent study is to explore a rapid, sensitive and selective Reversed Phase HPLC method for simultaneous quantification of steroidal hormones Levonorgestrel and Ethinylestradiol from drug products. Chromatographic separation of Levonorgestrel and Ethinylestradiol were achieved by Kromasil C8 column (4.6 mm u00d7 150 mm, 5 u00b5m) at 4.8 and 3.9 min by using 60:40 volume of acetonitrile and deionized water mobile phase at a flow rate of 1.0 ml/min at wavelength of 247 nm and 310 nm respectively. The injection volume was 100 u00b5L and the column temperature was maintained at 25u00b0C. The method was validated according to USP category I requirements which includes specificity, accuracy, precision, intermediate precision, linearity and range and robustness. The standard calibration curve were found linear (r2 >0.99) over the analytical range throughout the analysis day. Precision and intermediate precision was

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Stability indicating RP-HPLC method for simultaneous determination of Terlipressin in pure and pharmaceutical formulatio

A simple, selective, precise and stability indicating High Performance Liquid Chromatographic (HPLC) method of analysis of Terlipressin in pure and pharmaceutical dosage form was developed and validated. The chromatographic conditions comprised of a reversed-phase C18 column (250 x 4.6 mm), 5 µ with a mobile phase consisting of a mixture of Acetonitrilemonobasic potassium phosphate solution (35:65v/v) and pH adjusted to 3.5. Flow rate was 1.5 mL / min. Detection was carried out at 280 nm. The retention time of Terlipressin was 10.05 min. Terlipressin was subjected to acid and alkali hydrolysis, oxidation, photochemical degradation and thermal degradation. The linear regression analysis data for the calibration plots showed good linear relationship in the concentration range 2-12µg/ml. The value of correlation coefficient, slope and intercept were, 0.9995, 1848.2and 62.786, respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for specificity, linearity, precision, recovery, ruggedness and robustness. The drug undergoes degradation under acidic, basic, photochemical and thermal degradation conditions. All the peaks of degraded product were resolved from the active pharmaceutical ingredient with significantly different retention time. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one.

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Simultaneous estimation of lisinopril and hydrochlorthiazide in bulk, pharmaceutical dosage forms and in dissolution sam

The aim of the present work was to develop and validate a simple, efficient, economical RP-HPLC method for the simultaneous estimation of Lisinopril (LIS) and Hydrochlorothiazide (HCTZ) in bulk, dosage forms and in dissolution samples of LIS and HCTZ tablets. Chromatography was performed on Inertsil ODS 3 column (250 x 4.6mm, 5µm) with mobile phase containing 10mM Ammonium acetate: Acetonitrile (80:20% v/v) at a flow rate of 1mL/min and eluents were monitored at 220nm. The retention times of LIS and HCTZ were 3.7min and 7.6min respectively and showed a good linearity in the concentration range of 2-10µg/mL for LIS and 5-25ug/mL for HCTZ with a correlation coefficient of 0.998 and 0.996 respectively. The validation characteristics included specificity, linearity, and limit of detection, limit of quantification, precision, robustness and stability. Validation parameters fulfilled regulatory requirements in all cases. The percent recoveries were ranged in between 98-102, (RSD < 2). The developed HPLC method was successfully used for the simultaneous analysis of LIS and HCTZ in bulk, dosage forms and in dissolution samples of marketed LIS-HCTZ combination tablets.

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Reversed Phase High Pressure Liquid Chromatography Technique for Determination of Carbocisteine from Pharmaceutical Form

A simple, rapid and accurate high performance liquid chromatography method is described for determination of carbocisteine from pharmaceutical formulation. The separation of drug was achieved on (Amino Propyl Silane) APS-2 hypersil (250 X 4.6 mm) 5µ column. The mobile phase consisted a mixture of buffer and methanol (65:35 v/v). The buffer was a mixture of 0.02 M potassium dihydrogen phosphate monobasic and 0.01 M 1-hexane sulphonic acid sodium salt anhydrous. The detection was carried out at wavelength 210 nm. Buffer containing 0.02 M potassium dihydrogen phosphate monobasic and 0.01 M 1-hexane sulphonic acid sodium salt anhydrous used as a diluent. The method was validated for system suitability, linearity, accuracy, precision, robustness, stability of sample solution. The method has been successfully used to analyze carbocisteine from pharmaceutical formulation.

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Method development and validation for simultaneous estimation of Paracetamol and Etoricoxib in pharmaceutical dosage for

A RP-HPLC method was developed for simultaneous estimation of Paracetamol and Etoricoxib tablet formulation using Phenomenex Luna C18 column (250 mm × 4.6 mm id, 5 µm particle size) and a mobile phase of methanol : water (70:30 v/v), at flow rate 1.0 ml/min with UV detection at 235 nm. The retention time (tR) of Paracetamol and Etoricoxib found to be 3.07 and 5.72 min respectively. The proposed method was validated for system suitability, specificity, linearity, accuracy, precision, LOD, LOQ and robustness. All parameters were found to be within the acceptance limit. Linearity over the concentration range 5-30 µg/ml for both Paracetamol and Etoricoxib with regression coefficient (r2 ) 0.9998 and 0.9994 respectively. Limit of detection (LOD) found to be 0.10 µg/ml and 0.04 µg/ml whereas limit of quantitation (LOQ) found to be 0.33 µg/ml and 0.13 µg/ml for Paracetamol and Etoricoxib respectively. The accuracy of the proposed method was determined by recovery studies and found to be 99.74%- 101.25% and 99.08%-99.21% for Paracetamol and Etoricoxib respectively.

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Method development and validation of asenapine in bulk by RP-HPLC method

A simple, sensitive, precise and specific reverse phase high performance liquid chromatographic method was developed and validated for the determination of Asenapine in bulk and tablet dosage forms. It was found that the excipient in the tablet dosage forms does not interfere in the quantification of active drug by proposed method. The HPLC separation was carried out by reverse phase chromatography on Shimadzu HPLC, 10-At detector with hypersil ODS C18 Column 250 X 4.6 mm (particle size of 5µ) and constant flow pump. Rheodyne injector with 20µl loop with a mobile phase composed pure methanol at flow rate 1.0 ml/min. The detection was monitored at 270nm. The calibration curve for Tamsulosin was linear from 2-10mg/ml. The interday and intraday precision was found to be within limits. The proposed method has adequate sensitivity, reproducibility and specificity for the determination of Asenapine in bulk and its tablet dosage forms. LOD and LOQ for Asenapine were found to be 0.4329 and 0.1311.Accuracy (recoveries: 98.07-101.28%) and reproducibility were found to satisfactory.

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A rapid RP-HPLC method for the estimation of famciclovir in tablet dosage forms

A rapid and simple RP-HPLC chromatographic method has been developed for the estimation of famciclovir in API and tablet dosage form.

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Analytical Method Development and Validation of Teneligliptin by using RP HPLC with ICH Guidelines

Teneligliptin is drug used against type 2 diabetes mellitus and it is also a member of class of anti diabetic drugs known as dipeptidyl peptidase 4 inhibitors or gliptins . A simple, sensitive and accurate RP HPLC method has been developed for the determination of Teneligliptin in bulk formulation. The max of the Teneligliptin was found to be 246 nm in Methanol Phosphate buffer pH 3 70 30 v v . The method shows high sensitivity with linearity 10 to 50 u00b5-g ml regression equation y = 54647x 74133 r2 = 0.9968 . The various parameters according to ICH guidelines are followed for validating and testing of this method. The Detection limit and quantitation limit were found to be 0.109 u00b5-g ml 1 and 0.3305 u00b5-g ml1 in Methanol Phosphate buffer pH 3 70 30 v v respectively. The purity of tablet formulation was found to be 99.57 . The results demonstrated that the procedure is accurate, specific and reproducible RSD 2 , and also being simple, cheap and less time consuming and appropriate for the determination of Teneligliptin in bulk and pharmaceutical formulation. Dr. Pradnya Lokhande "Analytical Method Development and Validation of Teneligliptin by using RP-HPLC with ICH Guidelines" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-3 , April 2019, URL: https://www.ijtsrd.com/papers/ijtsrd21735.pdf Paper URL: https://www.ijtsrd.com/chemistry/chromatography/21735/analytical-method-development-and-validation-of-teneligliptin-by-using-rp-hplc-with-ich-guidelines/dr-pradnya-lokhande

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Analytical Method Development and Validation of Metformin Hydrochloride by using RP HPLC with ICH Guidelines

A simple and reproducible method was developed for Metformin MET by Reverse Phase High Performance Liquid Chromatography RP HPLC . Metformin was separated on C18 column 4.6x250mm, particle size 5u00b5-m , using combination of phosphate buffer with pH of 3.0 and Methanol at the UV detection of 238nm. Isocratic elution of phosphate buffer with pH of 3.0 and Methanol was used as a mobile phase with various ratios and flow rates, eventually 30 70 v v phosphate buffer with pH of 3.0 and Methanol was being set with the flow rate of 1mL min. The statistical validation parameters such as linearity, accuracy, precision, inter day and intra day variation were checked, assay studies of Metformin were within 98 to 102 indicating that the proposed method can be adoptable for quality control analysis of Metformin. Mr. Nilesh Nikam | Dr. Avish Maru | Dr. Anil Jadhav | Dr. Prashant Malpure "Analytical Method Development and Validation of Metformin Hydrochloride by using RP-HPLC with ICH Guidelines" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-3 , April 2019, URL: https://www.ijtsrd.com/papers/ijtsrd22812.pdf Paper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/22812/analytical-method-development-and-validation-of-metformin-hydrochloride-by-using-rp-hplc-with-ich-guidelines/mr-nilesh-nikam

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Determination of glycidol as a genotoxic impurity in linezolid drug substance by gas chromatography

A gas chromatographic method has been developed for the determination of Glycidol in Linezolid drug substance. The method was optimized based on the basis of peak shape and response of Glycidol. The method was validated as per ICH guideline in terms of LOD, LOQ, Method precision, accuracy and specificity. The LOD and LOQ values were found to be 3 ppm (3 u00b5g/ml) and 10 ppm (10 u00b5g/ml) respectively.

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References

VARIATIONS IN SAW PALMETTO FORMULATIONS IN THE US MARKET N. M. Enwerem 1 *, K. Kumar 1 , F . Ayorinde 2 , K. R. Scott 1 and A.K. Wutoh 1 1 Department of Pharmaceutical Sciences and 2 Department of Chemistry, Howard University,

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