scholarly journals Development and Validation of a HPLC-based Bioanalytical Method for Lorcaserin using Solid Phase Extraction and Application to a Pharmacokinetic Study in Rats

2018 ◽  
Vol 80 (2) ◽  
Author(s):  
Sadhana J Rajput ◽  
Mansi A Sathe ◽  
Swati D Patel
Keyword(s):  
Solid Phase Extraction ◽  
Pharmacokinetic Study ◽  
Solid Phase ◽  
Phase Extraction ◽  
Bioanalytical Method ◽  
Development And Validation

A Rapid and Sensitive Method for the Pharmacokinetic Study of Janumet (Sitagliptin and Metformin) Tablets by LC-MS/MS Coupled with Ion-Pair Solid Phase Extraction

2019 ◽  
Vol 15 (7) ◽  
pp. 776-784
Author(s):  
Xiaonian Han ◽  
Jing Wang ◽  
Jing Huang ◽  
Lirong Peng
Keyword(s):  
Solid Phase Extraction ◽  
Pharmacokinetic Study ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Ion Pair ◽  
Phase Extraction ◽  
Plasma Samples ◽  
Ionization Source ◽  
Tandem Mass Spectrometric

Background: As first-line treatments for diabetes, sitagliptin and metformin have been widely prescribed as a combination to enhance the therapeutic effect. Objective: To establish a methodology to simultaneously monitor the two drugs in vivo by a reversedphase Liquid Chromatography-Tandem Mass Spectrometric (LC-MS/MS) method. Methods: The two drugs were extracted from 50 μl human plasma by ion-pair solid phase extraction. The separation of the plasma samples was implemented on an Agilent Zorbax SB-CN column (150×4.6 mm, 5.0 µm). The mobile phase was the mixture (80:20, v/v) of methanol and 5.0 mM ammonium formate in water (pH 4.5). An ion trap spectrometer equipped with an electrospray ionization source was utilized to detect the elution in positive mode. Quantification of the analytes was achieved by Multiple Reaction Monitoring (MRM) using the transitions of m/z 408.3→235.1 for sitagliptin and m/z 130.1→ 60.2 for metformin. Results: Sitagliptin and metformin demonstrated good linearity among the range of 1.00-1000 ng/mL and 5.00-4000 ng/mL. The intra-day and inter-day investigations displayed precisions of ≤ 3.6% and an accuracy range of -7.5% to 6.0% for the two drugs. The mean recovery of the two drugs was 96.0% and 98.5%. Under mandatory storage conditions, both the drugs gave an acceptable stability. The throughput of the assay was found to be more than 100 plasma samples per day ascribed to the run time of 3.0 min for each sample. Conclusion: The developed method was successfully applied to a pharmacokinetic study for a fixeddose tablet formulation containing 50 mg sitagliptin and 500 mg metformin in 12 healthy volunteers.

scholarly journals Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva

2012 ◽  
Vol 62 (2) ◽  
pp. 211-220 ◽  
Author(s):  
Jasmina Tonic-Ribarska ◽  
Arlinda Haxhiu ◽  
Zoran Sterjev ◽  
Gordana Kiteva ◽  
Ljubica Suturkova ◽  
...  
Keyword(s):  
Valproic Acid ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Human Saliva ◽  
Hplc Method ◽  
Therapeutic Monitoring ◽  
Phase Extraction ◽  
Free Drug Concentration ◽  
Development And Validation

Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva A bioanalytical HPLC method with UV detection for the determination of the antiepileptic drug valproic acid in human saliva has been developed and validated. Saliva represents an alternative matrix for therapeutic monitoring of antiepileptic drugs due to the increasing interest in free drug concentration. The proposed method involved solid-phase extraction for sample preparation and yielded very good mean recoveries of 99.4 % and 97.9 % for valproic acid and IS, respectively. The calibration function for valproic acid was linear over the concentration range of 1.0-50.0 μg mL-1 (R2 = 0.9989). Within-run and between-run precision and accuracy were studied at four concentrations and RSDs were less than 7.3 and 2.2 %, while accuracy values were higher than 96.8 and 97.5 %, respectively. The described method provides sensitivity, linearity, precision, accuracy and is suitable for analyses of valproic acid in saliva samples.

scholarly journals Sample Preparation and Extraction in Small Sample Volumes Suitable for Pediatric Clinical Studies: Challenges, Advances, and Experiences of a Bioanalytical HPLC-MS/MS Method Validation Using Enalapril and Enalaprilat

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
Bjoern B. Burckhardt ◽  
Stephanie Laeer
Keyword(s):  
Sample Preparation ◽  
Solid Phase Extraction ◽  
Method Development ◽  
Matrix Effects ◽  
Solid Phase ◽  
Scale Up ◽  
Small Sample ◽  
Positive Pressure ◽  
Phase Extraction ◽  
Bioanalytical Method

In USA and Europe, medicines agencies force the development of child-appropriate medications and intend to increase the availability of information on the pediatric use. This asks for bioanalytical methods which are able to deal with small sample volumes as the trial-related blood lost is very restricted in children. Broadly used HPLC-MS/MS, being able to cope with small volumes, is susceptible to matrix effects. The latter restrains the precise drug quantification through, for example, causing signal suppression. Sophisticated sample preparation and purification utilizing solid-phase extraction was applied to reduce and control matrix effects. A scale-up from vacuum manifold to positive pressure manifold was conducted to meet the demands of high-throughput within a clinical setting. Faced challenges, advances, and experiences in solid-phase extraction are exemplarily presented on the basis of the bioanalytical method development and validation of low-volume samples (50 μL serum). Enalapril, enalaprilat, and benazepril served as sample drugs. The applied sample preparation and extraction successfully reduced the absolute and relative matrix effect to comply with international guidelines. Recoveries ranged from 77 to 104% for enalapril and from 93 to 118% for enalaprilat. The bioanalytical method comprising sample extraction by solid-phase extraction was fully validated according to FDA and EMA bioanalytical guidelines and was used in a Phase I study in 24 volunteers.

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