scholarly journals DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD OF 3, 4-METHYLENEDIOXY-N-ETHYLAMPHETAMINE IN DRIED BLOOD SPOT USING GAS CHROMATOGRAPHY-MASS SPEC-TROMETRY

2020 ◽  
pp. 94-99
Author(s):  
YAHDIANA HARAHAP ◽  
HANZEL IRAWAN ◽  
KUSWARDANI
Keyword(s):  
Flow Rate ◽  
Analytical Method ◽  
Method Development ◽  
Internal Standard ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Mass Spec ◽  
Validation Criteria ◽  
Development And Validation ◽  
Blood Spot

Objective: This study aims to develop and validate the analytical method to determine 3,4-Methylenedioxy-N-ethylamphetamine (MDEA) in DBS using GC-MS. Methods: This research used liquid-liquid micro-extraction for sample preparation and analysis was performed by GC-MS. In the method development, the optimized parameters were flow rate, column temperature, the spot of blood volume, % haematocrit, extraction and reconstitution of solvent volume, and sonication duration. Validation of the chosen method was performed based on EMEA bioanalytical guideline in 2011. Results: The optimum chromatographic conditions were obtained using HP-5 MS capillary columns (30 m x 0.25 mm i.d; 0.25 μm ); helium with 99.9% purity as a mobile phase; flow rate of 1.0 ml/min; column temperature was 250 °C; MS detection using 4 fragments at m/z values ​​of 72.00 and 44.00 for MDEA and 58.00 and 77.00 for ephedrine HCl as an internal standard. The DBS paper with the volume of blood spot 40 μl was then extracted using liquid-liquid micro-extraction with methanol 700 μl, sonication for 5 min, evaporated with nitrogen gas then reconstituted with 50 μl ethyl acetate. The validation results fulfilled the requirements based on the EMEA bioanalytical guideline in 2011. Conclusion: It can be concluded that the optimum condition of the analytical method by using GC-MS was obtained and fulfilled validation criteria with a range concentration of 15-250 ng/ml.

scholarly journals Development and Validation of LC Method for the Determination of Famciclovir in Pharmaceutical Formulation Using an Experimental Design

2008 ◽  
Vol 5 (1) ◽  
pp. 58-67 ◽  
Author(s):  
Srinivas Vishnumulaka ◽  
Narasimha Rao Medicherla ◽  
Allam Appa Rao ◽  
G. Edela Srinubabu
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Internal Standard Method ◽  
Intermediate Precision ◽  
Mobile Phase Flow Rate ◽  
Development And Validation

A rapid and sensitive RP-HPLC method with UV detection (242 nm) for routine analysis of famciclovir in pharmaceutical formulations was developed. Chromatography was performed with mobile phase containing a mixture of methanol and phosphate buffer (50:50,v/v) with flow rate 1.0 mL min−1. Quantitation was accomplished with internal standard method. The procedure was validated for linearity (correlation coefficient =0.9999), accuracy, robustness and intermediate precision. Experimental design was used for validation of robustness and intermediate precision. To test robustness, three factors were considered; percentage v/v of methanol in mobile phase, flow rate and pH; flow rate, the percentage of organic modifier and pH have considerable important effect on the response. For intermediate precision measure the variables considered were: analyst, equipment and number of days. The RSD value (0.86%,n=24) indicated an acceptable precision of the analytical method. The proposed method was simple, sensitive, precise, accurate and quick and useful for routine quality control.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Lansoprazole in Presence of Related Substances by QbD Approach

2021 ◽  
pp. 138-150
Author(s):  
Sachin B. Gholve ◽  
Jaiprakash N. Sangshetti ◽  
Omprakash G. Bhusnure ◽  
Ram S. Sakhare ◽  
Pratap H. Bhosale ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Drug Substance ◽  
Gastric Ulcers ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Rp Hplc

A rapid specific RP-HPLC method has been developed for the determination of Lansoprazole impurities in the drug substance. The control of pharmaceutical impurities is currently a critical issue in the pharmaceutical industry. The International Council for Harmonization (ICH) has formulated a workable guideline regarding the control of impurities. The objective of the recent study was to develop and validate a HPLC method for the quantitative determination of process-related impurities of Lansoprazole in pharmaceutical drug substance. Lansoprazole, 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl] methyl]-sulfinyl]- 1H-benzimidazole is an proton pump inhibitor used in the management of gastric ulcers. Chromatographic identification of the impurities was carried out by response surface methodology, applying a three-level Box Behnken design with three center points. Three factors selected were a mobile phase, flow rate, column temperature. Evaluation of the main factor, their interaction, and the quadric effect on peak resolution were done on Waters Symmetry C8, 250 x 4.6mm, 5µm column is used for the development of the method. The mobile phase consists of buffer and acetonitrile. The flow rate of the mobile phase was 1.0 ml/min with gradient elution. The column temperature is ambient and the detection wavelength is 235 nm. The injection volume was 10 µL. The method was validated as per ICH guidelines for linearity in the range of 50-150 µg/ml and the LOD & LOQ values obtained were 0.437×10-4 and 0.1325×10-3 µg/ml respectively which specifies the method's sensitivity. The proposed method was successfully used to determine the Lansoprazole impurities in drug substances.

Method Development and Validation For Determining Stability of Omadacycline In Biological Matrices By Liquid Chromatography–Mass Spectrometry

2019 ◽  
Vol 10 (04) ◽  
pp. 640-645
Author(s):  
Satya Prasad B ◽  
Jaya Kumari S
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Precipitation Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Mobile Phase Composition ◽  
Column Temperature ◽  
Standard Curve ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Source Flow

The validated protein precipitation method was applied for the estimation of Omadacycline (OM) in human plasma with Omadacycline-D9 (OMD9) as an internal standard (ISTD) by using HPLC-ESI-MS/MS. Zorbax Eclipse Plus C18, 2.1 x 50 mm, 3.5 μm, was selected as the analytical column. The column temperature was set at 45°C. Mobile phase composition was 0.1% formic acid: methanol (80:20 v/v). Source flow rate of 300 μL/min without a split. An injection volume of 10 μL. Omadacycline and Omadacycline-D9 mesylate were eluted at 1.2 ± 0.2 min, with a total run time of 3.0 min for each sample. The mass transitions of Omadacycline and Omadacycline-D9 obtained were m/z 557.6 ® 456.6 and 566.7 ® 456.6, respectively. The standard curve shows a correlation coefficient (r2) greater than 0.9983 with a range of 5.00 to 12000.00 pg/ml using the linear regression model.

scholarly journals Bioanalytical method development and validation of garenoxacin mesylate in human plasma by RP-HPLC

2019 ◽  
Vol 10 (2) ◽  
pp. 1314-1320
Author(s):  
Ajitha A ◽  
Sujatha K ◽  
Abbulu K
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Internal Standard ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation

A simple, precise, accurate Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method was developed for the estimation of Garenoxacin mesylate in human plasma using Ciprofloxacin Hydrochloride as an internal standard. Chromatographic conditions used are stationary phase Zorbax Eclipse XDB C18 (250x4.6 mm, 5m), Mobile phase 0.1% orthophosphoric acid and Acetonitrile in the ratio of 50:50 (% v/v) and flow rate was maintained at 1.0 ml/min, detection wavelength was 240 nm, injection volume of 50 µL and the column temperature was set to 30°C. The retention time of Garenoxacin mesylate was found to be 4.0 min. % Coefficient of Variation of the Garenoxacin mesylate was found to be 4.30. % Recovery was obtained as 98.97%. The linearity of the proposed method was established in the concentration range of 0.04 to 4 µg/ml (Correlation Coefficient = 0.999). The lower limit of quantification was 0.04 μg/ml (S/N Ratio 21) which reach the level drug possibly found in human plasma. Further, the reported method was validated as per the ICH guidelines and found to be well within the acceptable range.

Bioanalytical Method Development and Validation for the Determination of Vasopressin Receptor Antagonist Conivaptan in Mouse Plasma at NanoLevel and its Pharmacokinetic Application

2019 ◽  
Vol 15 (5) ◽  
pp. 591-598 ◽  
Author(s):  
Haitham Alrabiah ◽  
Ahmed Bakheit ◽  
Sabray Attia ◽  
Gamal A.E. Mostafa
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Vasopressin Receptor ◽  
Mouse Plasma ◽  
Precipitation Procedure ◽  
Validation Parameters ◽  
The Us ◽  
Method Development And Validation ◽  
Development And Validation

Background: Conivaptan inhibits two of vasopressin receptor (vasopressin receptor V1a and V2). Conivaptan is used for the treatment of hyponatremia, and in some instances, for the treatment of the heart failure. Methods: The present study aimed to develop a simple, sensitive, and accurate HPLC with ultraviolet detection for the assay of conivaptan (CON) in mouse plasma using bisoprolol as internal standard (IS). A precipitation procedure was used to extract CON and the IS from the mouse plasma. CON was chromatographically separated using a C18 analytical column at 25°C. The separation was carried out using a mixture of phosphate buffer (50 mM): acetonitrile (60: 40, v/v, pH 4.5) with a flow rate of 1.0 mL/min and detection was performed at 240 nm. Results: The assay was validated according to the US Food and Drug (FDA) guidelines. The method demonstrated linearity over a concentration range of 150 - 2000 ng/mL (correlation coefficient: r 2 = 0.9985). The mean recovery of CON from the mouse plasma was 101.13%. All validation parameters for CON were within the acceptable range. Conclusion: The investigated method has been shown to be suitable for estimating the CON in plasma samples, and this method is sensitive and highly selective, allowing the estimation of its concentrations up to the nano-scale. The suggested method was successfully used in a pharmacokinetic study of CON in mouse plasma.

scholarly journals RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms

2013 ◽  
Vol 49 (2) ◽  
pp. 359-366 ◽  
Author(s):  
Mustafa Çelebier ◽  
Tuba Reçber ◽  
Engin Koçak ◽  
Sacide Altinöz
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

Rivaroxaban, an anti-clotting medication, acts at a crucial point in the blood-clotting process and stops the formation of blood clots. In this study, RP-HPLC method was developed for the determination of rivaroxaban in tablets (Xarelto® (10 mg)). Phenomenex Luna 5 µm C18 100 Å LC Column (250 x 4.6 mm) was used at 40 ºC. Isocratic elution was performed with ACN:Water (55:45 v/v) mixture. The flow rate was 1.2 mL min-1 and UV detection was at 249 nm. Internal standard (Caffeine) and rivaroxaban were eluted within 2.21 and 3.37 minutes, respectively. The developed method was validated according to the ICH guidelines and found to be linear within the range 0.005 - 40.0 µg mL-1. The method was accurate, precise, robust and rapid. Thus, it was applied successfully for the quality control assay of rivaroxaban in tablet dosage form.

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