scholarly journals Development and Validation of UPLC-MS/MS Method for the Determination of Aripiprazole in Rat Plasma Using Liquid-Liquid Extraction: Pharmacokinetic and Bioequivalence Application

2020 ◽  
Vol 32 (10) ◽  
pp. 2671-2676
Author(s):  
Ashish Raghuvanshi ◽  
Urooj A. Khan ◽  
Uzma Parveen ◽  
Anshul Gupta ◽  
Gaurav K. Jain
Keyword(s):  
Internal Standard ◽  
Rat Plasma ◽  
Liquid Extraction ◽  
Single Step ◽  
Liquid Liquid Extraction ◽  
Validation Parameters ◽  
Tandem Mass Spectrometric ◽  
Liquid Chromatographic

A selective, simple, sensitive and rapid ultra-performance liquid chromatographic tandem mass spectrometric (UPLC-MS/MS) method for the detection of aripiprazole in rat plasma has been developed and validated using aripiprazole-D8 as internal standard (IS). A simple single step sample preparation process was accomplished by liquid-liquid extraction (LLE). The post-treatment samples were chromato-graphed and analyzed on a UPLC bridged ethyl hybrid (BEH) C-18 column using mobile phase composition of acetonitrile: 0.1% formic acid in water::70:30 (v/v). Aripiprazole was analyzed by MS detector in positive electrospray ionization mode (ESI). Multiple reactions monitoring (MRM) was employed to observed the transition for aripiprazole (m/z 448.35→285.09) and aripiprazole-D8 (m/z 456.2→293.2). The developed method was validated and found linear in the working range of 2-1025 ng/mL with correlation coefficient, r2 = 0.99951 and quantification limit of 2.02 ng/mL. All validation parameters were in accordance with the ICH guidelines and met the acceptance criteria. The method was found to be accurate (recovery, 97.07 to 103.64%, precise (% CV, 2.68 to 7.70%), rapid (run time 4 min) and specific. The validated method was successfully used for the determination of plasma concentration of aripiprazole after single oral administration in rats and hence could be useful for in vivo pharmacokinetic study and bioequivalence testing of aripiprazole formulations.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE DETERMINATION OF ALVIMOPAN IN RAT PLASMA

2018 ◽  
Vol 10 (10) ◽  
pp. 124
Author(s):  
Devi Ramesh ◽  
Mohammad Habibuddin
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
The United States ◽  
Hplc Method ◽  
Liquid Extraction ◽  
Pharmacokinetic Parameters ◽  
Dihydrogen Phosphate ◽  
Liquid Liquid Extraction ◽  
Validation Parameters

Objective: The present investigation demonstrates a simple, sensitive and accurate high pressure liquid chromatographic (HPLC) method for the determination of alvimopan (AMP) in rat plasma.Methods: The chromatographic separation was achieved within 10 min by using acetonitrile: potassium dihydrogen phosphate buffer pH 3.0 adjusted with orthophosphoric acid (50:50) as mobile phase on Altima Grace Smart C-18 column (5μ; 250 × 4.6 mm) at a flow rate of 1.0 ml/min with injection volume 50 µl. The drug was extracted from plasma by liquid-liquid extraction using a mixture of methanol: acetonitrile (50:50) as a solvent. The retention times of drug and internal standard were found to be 5.17 and 6.74 min, respectively. This method was validated as per the United States Food and Drug Administration (US-FDA) guidelines.Results: The results of the validation parameters were found to be within the acceptance limits. The method was linear in the concentration range from 5-1000 ng/ml (r2= 0.9998), and the extraction recovery was found to be 78.71±3.86% for AMP. The lower limit of quantification was found to be 5ng/ml, and the stability of recovered samples at different conditions was found to be more than 95%.Conclusion: The developed method possess good selectivity, specificity, there was no interference found in the plasma blanks at retention times of AMP and Internal Standard (IS). We found a good correlation between the peak area and concentration of the drug under prescribed conditions. Furthermore, the method can also be used to estimate the pharmacokinetic parameters of AMP.Keywords: Alvimopan, Liquid-liquid extraction, Method development, Matrix effect, Plasma, Recovery, Stability, Validation

scholarly journals Simultaneous Determination of Docetaxel and Celecoxib in Porous Microparticles and Rat Plasma by Liquid-Liquid Extraction and HPLC with UV Detection: in vitro and in vivo Validation and Application

2020 ◽  
Vol 23 ◽  
pp. 289-303
Author(s):  
Elham Ziaei ◽  
Jaber Emami ◽  
Moloud Kazemi ◽  
Mahboubeh Rezazadeh
Keyword(s):  
Internal Standard ◽  
Rat Plasma ◽  
Liquid Extraction ◽  
Uv Detection ◽  
Pharmacokinetic Studies ◽  
Liquid Liquid Extraction ◽  
Porous Microparticles ◽  
Limit Of Quantitation

Purpose: A simple, rapid, sensitive, and reliable HPLC method with UV detection was developed and validated for simultaneous quantitation of docetaxel and celecoxib and paclitaxel for dissolution characterization and pharmacokinetic studies. Methods: The HPLC assay was performed isocratically on a reversed-phase C18 μ-Bondapack column using a mobile phase of acetonitrile:water (45:55, v/v) at a flow rate of 1.2 mL/min, and the analytes were detected at 230 nm. Paclitaxel was used as an internal standard for analysis of plasma samples following simple liquid-liquid extraction with n-hexane:isoamyl alcohol (97:3). The method was validated for specificity, linearity, sensitivity, precision, accuracy, robustness, and in vitro-in vivo application. Results: The retention times for docetaxel, paclitaxel, and celecoxib were 10.94, 12.4, and 16.81 min, respectively. The standard curves covering 0.1-1 μg/mL and 0.05-4 μg/mL were linear using dissolution medium and rat plasma, respectively. The limit of quantitation of the method was 50 ng/mL using 100 μL of rat plasma sample and injection of 50 μL of the residue. Within- and between-day precision and accuracy did not exceed 16.86% and 12.10%, respectively. This validated method was successfully used to quantify docetaxel and celecoxib simultaneously in the release study of docetaxel-celecoxib -loaded porous microparticles and pharmacokinetics studies. The methods were found to be simple, specific, precise, accurate, and reproducible. In this study, paclitaxel was used as the internal standard while dexamethasone, flutamide, and budesonide proved suitable alternative as an internal standard. Conclusion: Since docetaxel and celecoxib could be co-administered for the treatment of a wide range of cancers such as non-small cell lung carcinoma, the developed method is particularly advantageous for routine therapeutic drug monitoring and pharmacokinetic studies of these drugs.

DETERMINATION OF URANIUM IN FLOTATION CONCENTRATES AND IN LEACH LIQUORS BY X-RAY FLUORESCENCE

1959 ◽  
Vol 37 (1) ◽  
pp. 20-28 ◽  
Author(s):  
G. L. Smithson ◽  
R. L. Eager ◽  
A. B. VanCleave
Keyword(s):  
Direct Measurement ◽  
Pilot Plant ◽  
Internal Standard ◽  
Liquid Extraction ◽  
X Ray ◽  
Liquid Liquid Extraction ◽  
Northern Saskatchewan ◽  
Plant Operations ◽  
Time Required

X-Ray fluorescence has been applied to the analysis of flotation concentrates obtained from pegmatitic uranium ores occurring in Northern Saskatchewan. Approximate uranium analyses can be obtained by direct measurement on flotation concentrates but more accurate results are obtained by using an internal standard such as strontium or yttrium. The time required for an analysis, as compared to that of conventional chemical or fluorimetric methods, is considerably reduced and flotation pilot plant operations can therefore be more effectively controlled. The method has been extended to include the analysis of sulphate leach liquors obtained from the leaching of pegmatitic ores and their flotation concentrates. Organic phases obtained in liquid – liquid extraction studies can also be rapidly analyzed for uranium by X-ray fluorescence.

Simultaneous determination of haloperidol and its reduced metabolite in serum and plasma by isocratic liquid chromatography with electrochemical detection.

1983 ◽  
Vol 29 (4) ◽  
pp. 624-628 ◽  
Author(s):  
E R Korpi ◽  
B H Phelps ◽  
H Granger ◽  
W H Chang ◽  
M Linnoila ◽  
...  
Keyword(s):  
Psychiatric Patients ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Reversed Phase ◽  
Reduced Haloperidol ◽  
Liquid Liquid Extraction ◽  
Liquid Chromatographic Method ◽  
The Central Nervous System ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic method for simultaneous quantification of haloperidol and its reduced metabolite in plasma and serum. Haloperidol and reduced haloperidol are concentrated from blood samples by liquid/liquid extraction into a hexane/isoamyl alcohol mixture, with chlorohaloperidol as the internal standard. For chromatographic separation we used a reversed-phase cyano-bonded column and a mobile phase of pH 6.8 phosphate buffer/acetonitrile (55/45 by vol). Haloperidol and its reduced metabolite are detected electrochemically at +0.90 V potential between the working and reference electrodes. As little as 0.5 ng per injection is detectable. Within- and between-day CVs for determinations of haloperidol and reduced haloperidol ranged from 4 to 7% each at a concentration of 10 micrograms/L. Haloperidol concentrations measured by this method correlated well with those by gas-chromatography with nitrogen-sensitive detector and by radioimmunoassay. The present method can be used to study the effects of haloperidol on the central nervous system. It is simple enough for use in clinical laboratories that are monitoring haloperidol concentrations in the blood of psychiatric patients.

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