scholarly journals Automated On-Line Solid-Phase Extraction Coupled with HPLC for Measurement of 5-Hydroxyindole-3-acetic Acid in Urine

2005 ◽  
Vol 51 (9) ◽  
pp. 1698-1703 ◽  
Author(s):  
Erik J Mulder ◽  
Alida Oosterloo-Duinkerken ◽  
George M Anderson ◽  
Elisabeth GE De Vries ◽  
Ruud B Minderaa ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Solid Phase Extraction ◽  
Urinary Excretion ◽  
Extraction Method ◽  
Solid Phase ◽  
Internal Standard ◽  
Carcinoid Tumors ◽  
Phase Extraction ◽  
Automated Method ◽  
On Line

Abstract Background: Quantification of 5-hydroxyindole-3-acetic acid (5-HIAA) in urine is useful in diagnosing and monitoring of patients with carcinoid tumors and in the study of serotonin (5-hydroxytryptamine) metabolism in various disorders. We describe an automated method that incorporates on-line solid-phase extraction (SPE) and HPLC to measure urinary 5-HIAA. Methods: Automated prepurification of urine was accomplished with HySphere-resin GP SPE cartridges containing strong hydrophobic polystyrene resin. The analyte (5-HIAA) and internal standard [5-hydroxyindole-3-carboxylic acid (5-HICA)] were eluted from the SPE cartridge, separated by reversed-phase HPLC, and detected fluorometrically with a total cycle time of 20 min. Urinary excretion of 5-HIAA was measured in a group of patients with known and suspected carcinoid tumors (n = 63) and in 20 patients with autism. Results: The internal standard (5-HICA) and 5-HIAA were recovered in high yields (87.2%–114%). Within- and between-series CVs for the measurement of 5-HIAA in urine ranged from 1.2% to 3.9% and 3.2% to 7.6%, respectively. For urine samples from patients with known or suspected carcinoid tumors, results obtained by the automated method were highly correlated (r = 0.988) with those from an established manual extraction method. For samples from autistic patients, urinary excretion of 5-HIAA was similar to that reported for healthy individuals. Conclusion: This SPE-HPLC method demonstrated lower imprecision and time per analysis than the manual solvent extraction method.

Automated method to determine pharmaceutical compounds in wastewater using on-line solid-phase extraction coupled to LC-MS/MS

2021 ◽  
Author(s):  
César Augusto Marasco Júnior ◽  
Bianca Ferreira da Silva ◽  
Rafaela Silva Lamarca ◽  
Paulo Clairmont Feitosa de Lima Gomes
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Pharmaceutical Compounds ◽  
Phase Extraction ◽  
Automated Method ◽  
On Line

scholarly journals Profiling of Tryptophan-related Plasma Indoles in Patients with Carcinoid Tumors by Automated, On-Line, Solid-Phase Extraction and HPLC with Fluorescence Detection

2001 ◽  
Vol 47 (10) ◽  
pp. 1811-1820 ◽  
Author(s):  
Ido P Kema ◽  
Wim G Meijer ◽  
Gert Meiborg ◽  
Bert Ooms ◽  
Pax H B Willemse ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Patient Group ◽  
Solid Phase ◽  
Platelet Rich Plasma ◽  
Single Component ◽  
Carcinoid Tumors ◽  
Phase Extraction ◽  
Healthy Controls ◽  
On Line ◽  
Plasma Serotonin

Abstract Background: Profiling of the plasma indoles tryptophan, 5-hydroxytryptophan (5-HTP), serotonin, and 5-hydroxyindoleacetic acid (5-HIAA) is useful in the diagnosis and follow-up of patients with carcinoid tumors. We describe an automated method for the profiling of these indoles in protein-containing matrices as well as the plasma indole concentrations in healthy controls and patients with carcinoid tumors. Methods: Plasma, cerebrospinal fluid, and tissue homogenates were prepurified by automated on-line solid-phase extraction (SPE) in Hysphere Resin SH SPE cartridges containing strong hydrophobic polystyrene resin. Analytes were eluted from the SPE cartridge by column switching. Subsequent separation and detection were performed by reversed-phase HPLC combined with fluorometric detection in a total cycle time of 20 min. We obtained samples from 14 healthy controls and 17 patients with metastasized midgut carcinoid tumors for plasma indole analysis. In the patient group, urinary excretion of 5-HIAA and serotonin was compared with concentrations of plasma indoles. Results: Within- and between-series CVs for indoles in platelet-rich plasma were 0.6–6.2% and 3.7–12%, respectively. Results for platelet-rich plasma serotonin compared favorably with those obtained by single-component analysis. Plasma 5-HIAA, but not 5-HTP was detectable in 8 of 17 patients with carcinoid tumors. In the patient group, platelet-rich plasma total tryptophan correlated negatively with platelet-rich plasma serotonin (P = 0.021; r = −0.56), urinary 5-HIAA (P = 0.003; r = −0.68), and urinary serotonin (P <0.0001; r = −0.80). Conclusions: The present chromatographic approach reduces analytical variation and time needed for analysis and gives more detailed information about metabolic deviations in indole metabolism than do manual, single-component analyses.

Development of an on-line solid phase extraction method based on new functionalized magnetic nanoparticles. Use in the determination of mercury in biological and sea-water samples

Talanta ◽  
2016 ◽  
Vol 153 ◽  
pp. 228-239 ◽  
Author(s):  
Elisa Vereda Alonso ◽  
M.M. López Guerrero ◽  
Pilar Colorado Cueto ◽  
José Barreno Benítez ◽  
José Manuel Cano Pavón ◽  
...  
Keyword(s):  
Magnetic Nanoparticles ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
Extraction Method ◽  
Sea Water ◽  
Solid Phase ◽  
Phase Extraction ◽  
Functionalized Magnetic Nanoparticles ◽  
On Line

scholarly journals An on-line solid phase extraction method coupled with UHPLC-MS/MS for the determination of steroid hormone compounds in treated water samples from waste water treatment plants

2015 ◽  
Vol 7 (14) ◽  
pp. 5996-6005 ◽  
Author(s):  
Rayco Guedes-Alonso ◽  
Zoraida Sosa-Ferrera ◽  
José Juan Santana-Rodríguez
Keyword(s):  
Solid Phase Extraction ◽  
Extraction Method ◽  
Solid Phase ◽  
Steroid Hormone ◽  
Waste Water Treatment ◽  
Phase Extraction ◽  
Waste Waters ◽  
Water Treatment Plants ◽  
On Line

An on-line solid phase extraction coupled with UHPLC-MS/MS method for the determination of fourteen hormones in waste waters has been developed.

scholarly journals Determination of Ranitidine in Human Plasma by SPE and ESI-LC-MS/MS for Use in Bioequivalence Studies

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Karini B. Bellorio ◽  
Maria Isabel R. Alves ◽  
Nelson R. Antoniosi Filho
Keyword(s):  
Solid Phase Extraction ◽  
Human Plasma ◽  
Extraction Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Internal Standard ◽  
Phase Extraction ◽  
Good Separation ◽  
Limit Of Quantification

A method for determining ranitidine in human plasma by ESI-LC-MS/MS was validated, using propranolol as internal standard. The extraction method used was solid phase extraction (SPE). Chromatographic separation was performed in a Chromolith C18 (50 mm × 4.6 mm i.d.) analytical column, which provided good separation of ranitidine and propranolol peaks with an analysis time of 2.5 minutes. Extraction yields of 94.4% for ranitidine and 89.4% for the internal standard were obtained. The lower limit of quantification (LLOQ) was 3.00 ng/mL, and limit of detection (LOD) was 0.05 ng/mL, with linearity ranging from 3.00 to 500 ng/mL. The results, thus, showed that this method is suitable for application in bioequivalence studies of ranitidine in human plasma.

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