Foodstuffs. Determination of okadaic acid in mussels. HPLC method with solid phase extraction clean-up, derivatization and fluorimetric detection

2004 ◽  
Keyword(s):  
Solid Phase Extraction ◽  
Okadaic Acid ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Fluorimetric Detection

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 HPLC determination of hydrochlorothiazide in urine after solid-phase extraction

2005 ◽  
Vol 51 ◽  
pp. 23-28 ◽  
Author(s):  
Violeta Ivanova ◽  
Dragica Zendelovska ◽  
Marina Stefova
Keyword(s):  
Particle Size ◽  
Solid Phase Extraction ◽  
Mobile Phase ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Hplc Separation ◽  
Isocratic Elution ◽  
Extraction Recovery

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.

Development of an HPLC method for the determination of nifedipine in human plasma by solid-phase extraction

2006 ◽  
Vol 839 (1-2) ◽  
pp. 85-88 ◽  
Author(s):  
Dragica Zendelovska ◽  
Suzana Simeska ◽  
Olgica Sibinovska ◽  
Elena Kostova ◽  
Kalina Miloševska ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Human Plasma ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction

scholarly journals Determination of 11 Phthalate Esters in Beverages by Magnetic Solid-Phase Extraction Combined with High-Performance Liquid Chromatography

2019 ◽  
Vol 102 (5) ◽  
pp. 1624-1631 ◽  
Author(s):  
Shuo Yin ◽  
Yi Yang ◽  
Danni Yang ◽  
Yongxin Li ◽  
Yang Jiang ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Phthalate Esters ◽  
Magnetic Solid Phase Extraction ◽  
Hplc Method ◽  
Phase Extraction ◽  
Established Method ◽  
Strong Adsorption ◽  
Magnetic Solid

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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