Rapid and Sensitive Quantitation of Inorganic Anions in Olive Oil by Coupling Reversed-Phase Dispersive Liquid–Liquid Microextraction and Ion Chromatography

Author(s):  
Sahar Rezaeinejad ◽  
Payman Hashemi
Toxins ◽  
2021 ◽  
Vol 13 (1) ◽  
pp. 57
Author(s):  
Ainhoa Oller-Ruiz ◽  
Natalia Campillo ◽  
Manuel Hernández-Córdoba ◽  
Javier Gilabert ◽  
Pilar Viñas

The use of dispersive liquid–liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 µL of chloroform were injected into 12 mL of sample. The enriched organic phase, once evaporated and reconstituted in methanol, was analyzed by reversed-phase liquid chromatography with triple-quadrupole tandem mass spectrometry. A central composite design multivariate method was used to optimize the interrelated parameters affecting DLLME efficiency. The absence of any matrix effect in the samples allowed them to be quantified against aqueous standards. The optimized procedure was validated by recovery studies, which provided values in the 82–123% range. The detection limits varied between 0.2 and 5.7 ng L−1, depending on the analyte, and the intraday precision values were in the 0.1–7.5% range in terms of relative standard deviation. Ten water samples taken from different points of the Mar Menor lagoon were analyzed and were found to be free of the studied toxins.


2021 ◽  
Vol 76 (11) ◽  
pp. 1305-1311
Author(s):  
E. V. Dmitrieva ◽  
A. Z. Temerdashev ◽  
A. K. Osipova

Abstract A method is proposed for the determination of some ketosteroids in human urine, including enzymatic hydrolysis using β-glucuronidase from E. coli followed by dispersive liquid-liquid microextraction, derivatization of analytes with hydroxylamine, and detection by reversed-phase ultra-HPLC–quadrupole time-of-flight mass spectrometry. Optimization of extraction and derivatization conditions of the studied compounds made it possible to find that the highest recoveries were achieved using an acetone–chloroform mixture as a dispersant and an extractant, and the completeness of the derivatization reaction was achieved by thermostating the sample at 70°C for 90 min. The proposed method has high sensitivity (limits of detection in the range of 0.1–0.25 ng/mL) and a wide linearity range.


Sign in / Sign up

Export Citation Format

Share Document