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.

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.

Bioanalytical Method Development and Validation of Doravirine, Lamavudine and Tenofovir Disoproxil Fumarate using HPLC in Human Plasma

2021 ◽  
pp. 4087-4091
Author(s):  
Marakatham S. ◽  
Shanmugapandiyan P.
Keyword(s):  
Human Plasma ◽  
Tenofovir Disoproxil Fumarate ◽  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
Stability Study ◽  
Dihydrogen Phosphate ◽  
Bioanalytical Method ◽  
Method Development And Validation ◽  
Development And Validation

A novel, simple and sensitive bioanalytical method was developed for estimation of Doravirine, Lamavudine and tenofovir disoproxil fumarate in human plasma with daclatasvir as internal standard. The method was developed using alliance HPLC using Phenomenex C18 (150mm x 4.6mm, 5m) column with mobile phase of 0.01N Potassium dihydrogen phosphate pH (3.5): Acetonitrile (60:40) at flow rate of 1.0ml/min. Detection wavelength was found to be 277nm. The linearity range for doravirine, lamuvidine and Tenfovir was 50-2000ng/ml, 125-5000ng/ml and 20-800ng/ml. Correlation coefficient was 0.999. The method was validated and stability study was carried out as per FDA guidelines.

SENSITIVE BIO ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF VENETOCLAX IN HUMAN PLASMA BY LC-ESI-MS/MS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (06) ◽  
pp. 32-38
Author(s):  
H. Potluri ◽  
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Liquid Liquid Extraction ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Method Development And Validation ◽  
Development And Validation

A specific and sensitive method of liquid chromatography–tandem mass spectrometry was demonstrated for the experimental determination of venetoclax in human plasma utilising venetoclax-D8 as an internal standard. The column Xbridge C18, 50 × 4.6mm, 5 µm was used for attaining chromatographic separation by utilising 10mM ammonium formate and methanol as isocratic mobile phase in the composition ratio of 20:80 (V/V). The flow-rate selected was 0.7ml/min. Venetoclax and venetoclax-D8 are identified in multiple reaction monitoring (MRM) positive mode with proton adducts at m/z 869.53 →553.21 and m/z 877.14 → 553.23, respectively. For the successful extraction of drug as well as internal standard, liquid-liquid extraction technique was efficiently utilised. The developed technique was established in a linear concentration range of 5.0-5000.0 pg/ml along with correlation coefficient (r2) of 0.9994. Intra and inter-day precisions were found to be 0.7 to 1.90% and 0.7 to 2.0 % for venetoclax and venetoclax-D8, respectively. Accuracy was found to be within 98.6 to 101.99% and 99.17 to 101.14 % for venetoclax and venetoclax-D8, respectively. It was observed that throughout the bench top studies, post-operative stability studies and freeze-thawing cycles, venetoclax retained stability.

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 HPLC-UV Method Development and Validation of Potato Sprout Inhibitor 1,4-Dimethylnaphthalene Using Different Systems

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Nidhal S. Mohammed ◽  
T. H. Flowers ◽  
H. J. Duncan
Keyword(s):  
Environmental Samples ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Reversed Phase ◽  
Potato Sprout ◽  
Method Development And Validation ◽  
Residue Levels ◽  
Development And Validation

1,4-Dimethylnaphthalene (1,4-DMN) is effective sprout suppressant used in potato stores in many countries in the world. High residue levels of this compound on the potatoes and in other environmental samples are considered for human health and environmental risks. Determination of the residue requires specific analytical methods to be developed and validated. In this study, HPLC-UV was selected for validating a separation method based on reversed phase for the analysis of 1,4-DMN using 2-methylnaphthalene (2-MeN) as internal standard testing three HPLC systems. Under the same chromatographic conditions, all three systems achieved good separation on a Jones column (Hypersil ODS 5 μm, 250 mm × 4.6 mm) at ambient temperature isocratically using 70% acetonitrile as mobile phase at a flow rate of 1.5 mL min−1, 20 μL injection volume, a run time of 10 min, and a detection wavelength of 228 nm. All three systems showed high precision, good linearity, and low limit of detection (LOD) and quantification (LOQ); particularly, the SpectraSERIES UV100-autosampler system offered lower values of LOD (0.001–0.004 μg mL−1) and LOQ (0.002–0.013 μg mL−1) for both compounds. This system can be used for the quantitative determination of 1,4-DMN residue in potato and environmental samples.

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