scholarly journals HPLC Method with Solid-Phase Extraction for Determination of (R)- and (S)-Ketoprofen in Plasma without Caffeine Interference: Application to Pharmacokinetic Studies in Rats

2013 ◽  
Vol 52 (10) ◽  
pp. 1204-1210 ◽  
Author(s):  
Francisco Javier López-Muñoz ◽  
Nancy Vara Gama ◽  
Olivia Soria-Arteche ◽  
Marcela Hurtado y de la Peña ◽  
Adriana Miriam Domínguez-Ramírez ◽  
...  
2012 ◽  
Vol 62 (2) ◽  
pp. 211-220 ◽  
Author(s):  
Jasmina Tonic-Ribarska ◽  
Arlinda Haxhiu ◽  
Zoran Sterjev ◽  
Gordana Kiteva ◽  
Ljubica Suturkova ◽  
...  

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.


2005 ◽  
Vol 51 ◽  
pp. 23-28 ◽  
Author(s):  
Violeta Ivanova ◽  
Dragica Zendelovska ◽  
Marina Stefova

A simple, rapid and precise HPLC method has been developed for the assay of hydrochlorothiazide in urine. The clean-up of the urine samples was carried out by solid-phase extraction using HLB cartridges. Extraction recovery was 94.00-100.28 %. HPLC separation was performed with isocratic elution on Hypersil BDS C18 column (100 x 4.0 mm I.D., 3 µm particle size) protected with appropriate guard column. The mobile phase was 18 % acetonitrile and 0.025 mol/L solution of KH2PO4, pH 4 at flow rate of 0.3 mL/min. Detection of the substances was performed at 220 nm. The calibration curves were linear in the range of 2-50 µg/mL. The developed method is validated by checking its accuracy, precision and stability. The detection limit is 2 µg/mL hydrochlorothiazide. The method is proved to be convenient for routine analysis of hydrochlorothiazide in urine.


2006 ◽  
Vol 839 (1-2) ◽  
pp. 85-88 ◽  
Author(s):  
Dragica Zendelovska ◽  
Suzana Simeska ◽  
Olgica Sibinovska ◽  
Elena Kostova ◽  
Kalina Miloševska ◽  
...  

2000 ◽  
Vol 46 (6) ◽  
pp. 837-842 ◽  
Author(s):  
Nina Isoherranen ◽  
Stefan Soback

Abstract Background: Gentamicin is an aminoglycoside antibiotic complex containing gentamicins C1, C1a, and C2. Few methods have been described for analysis of the three gentamicin components separately in biological fluids, and none has been used in pharmacokinetic studies. Determination of the three gentamicins separately may have pharmacokinetic and toxicological implications. The present study describes development of an HPLC method for the analysis of gentamicin C1, C1a, and C2 components in plasma and urine. Methods: The three components were isolated by preparative chromatography and their identities verified by thin-layer chromatography, HPLC, mass spectrometry, nuclear magnetic resonance spectroscopy, and melting point determination. The gentamicins were extracted from the biological matrix by use of Tris buffer and polymer phase solid-phase extraction. Derivatization was carried out in the solid-phase extraction cartridge with 1-fluoro-2,4-dinitrobenzene. The 2,4-dinitrophenyl derivatives were separated with reversed-phase HPLC and quantified by the ultraviolet absorbance at 365 nm. Results: The detector response was linear from the limit of quantification to 50 mg/L for the individual components. The limit of quantification was 0.07 mg/L for gentamicin C1 and 0.1 mg/L for gentamicins C2 and C1a. The recovery of the gentamicin components was 72% from plasma and 98% from urine. The method was validated for human and dog plasma and urine. Conclusions: The method was repeatable and enabled the analysis of gentamicins C1, C1a, and C2 in plasma and urine in concentrations covering the therapeutic range of the drug, thus being suitable for therapeutic drug monitoring and pharmacokinetic studies.


2019 ◽  
Vol 102 (5) ◽  
pp. 1624-1631 ◽  
Author(s):  
Shuo Yin ◽  
Yi Yang ◽  
Danni Yang ◽  
Yongxin Li ◽  
Yang Jiang ◽  
...  

Abstract Background: Beverages can be easily contaminated by phthalate esters (PAEs) during the production, bottling, and transportation processes. It is necessary to determine the contamination level in beverages for assessment of human exposure. Objective: In this study, magnetic solid-phase extraction (MSPE) was combined with HPLC for the determination of 11 PAEs in beverages. Methods: Self-synthesized magnetic multiwalled carbon nanotubes (m-MWCNTs) were used as the adsorbent for PAE extraction. To extract the PAEs, an appropriate amount of m-MWCNTs and NaCl was added to the beverage sample. The mixture was mixed on a vortex mixer, the magnetic sorbent was collected with the aid of a magnet, and the supernatant was removed. Then, the analytes were eluted with n-hexane–acetone (1+1, v/v). Finally, the eluent was analyzed by the HPLC method. The separation was accomplished on a Phenomenex Luna-C18 column (250 × 4.6 mm, 5 μm), and the detection wavelength was set at 225 nm. Results: The linear ranges of the method were 2–300 μg/L with correlation coefficients greater than 0.9981. The LOD and LOQ were in the range of 0.659–5.33 × 10–2 μg/L and 2.20–17.8 × 10–2 μg/L, respectively. The recoveries of the method ranged from 79.8 to 114%, with the relative SDs less than 15.8%. The established method has been successfully applied for the determination of 11 PAEs in mineral water, carbonated soft drink, tea beverage, and fruit juice samples. PAEs were detected at 0.246–34.3 μg/L in these samples. Conclusions: The m-MWCNTs are the satisfactory sorbent for MSPE because of their strong adsorption capacity for PAEs. The established MSPE-HPLC method is rapid, easy, sensitive, green, and cost-effective. It can be applied to the analysis of trace PAEs in plastic bottled beverages. Highlights: Three magnetic nanoparticles (MNPs), including Fe3O4 MNPs, m-MWCNTs, and magnetic graphene oxide, were synthesized, and m-MWCNTs were chosen as the sorbent of MSPE for PAE extraction because of their strong adsorption capacity for PAEs. An MSPE–HPLC method has been developed for the analysis of 11 phthalates in plastic bottled beverages. The established method was successfully applied to the analysis of 11 phthalates in four types of beverage samples.


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