Determination of triazine herbicides in seaweeds: Development of a sample preparation method based on Matrix Solid Phase Dispersion and Solid Phase Extraction Clean-up

Talanta ◽  
2014 ◽  
Vol 121 ◽  
pp. 194-198 ◽  
Author(s):  
N. Rodríguez-González ◽  
M.J. González-Castro ◽  
E. Beceiro-González ◽  
S. Muniategui-Lorenzo ◽  
D. Prada-Rodríguez
Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2350
Author(s):  
Jianing Zhang ◽  
Fengjie Yu ◽  
Yunmin Tao ◽  
Chunping Du ◽  
Wenchao Yang ◽  
...  

In the present work, a novel sample preparation method, micro salting-out assisted matrix solid-phase dispersion (μ-SOA-MSPD), was developed for the determination of bisphenol A (BPA) and bisphenol B (BPB) contaminants in bee pollen. The proposed method was designed to combine two classical sample preparation methodologies, matrix solid-phase dispersion (MSPD) and homogenous liquid-liquid extraction (HLLE), to simplify and speed-up the preparation process. Parameters of μ-SOA-MSPD were systematically investigated, and results indicated the significant effect of salt and ACN-H2O extractant on the signal response of analytes. In addition, excellent clean-up ability in removing matrix components was observed when primary secondary amine (PSA) sorbent was introduced into the blending operation. The developed method was fully validated, and the limits of detection for BPA and BPB were 20 μg/kg and 30 μg/kg, respectively. Average recoveries and precisions were ranged from 83.03% to 94.64% and 1.76% to 5.45%, respectively. This is the first report on the analysis of bisphenol contaminants in bee pollen sample, and also on the combination of MSPD and HLLE. The present method might provide a new strategy for simple and fast sample preparation of solid and semi-solid samples.


2003 ◽  
Vol 86 (4) ◽  
pp. 729-736 ◽  
Author(s):  
Aldo Laganà ◽  
Alessandro Bacaloni ◽  
Maryanna Castellano ◽  
Roberta Curini ◽  
Ilaria De Leva ◽  
...  

Abstract A new method based on matrix solid-phase dispersion (MSPD) on-line with a solid-phase extraction (SPE) cleanup process followed by liquid chromatography with tandem mass spectrometry (LC/MS/MS) is presented for the determination of 3 macrocyclic lactone mycotoxins in fish tissues: zearalenone, α-zearalenol, and β-zearalenol. The sample was prepared in a device that used a reversed-phase material (C18) or a normal-phase material (neutral alumina) as a matrix dispersing agent, and a graphitized carbon black cartridge was used for sequential cleanup by SPE. LC/MS/MS was used for selective determination. Isocratic elution with acetonitrile–methanol–water was used for LC separation; for MS/MS, 2 types of interfaces (a pneumatically assisted electrospray ionization interface or an atmospheric pressure chemical ionization interface) were evaluated and compared in terms of the intensity of the total ion current produced by each analyte. The use of highly selective MSPD on-line with SPE for sample preparation before analysis allowed the removal of interfering matrix compounds `present in tissue extracts that would otherwise cause severeionization suppression of zearalenone and its metabolites during the ionization process. Average recoveries at 100 ng/g were between 83 and 103% with C18 and ≥67% with neutral alumina; the relative standard deviations were <11% with C18 and <18% with alumina. The limits of detection ranged from 0.1 to 1.0 ng/g. Sample preparation is simple to perform, no special technical equipment is required, and solvent volumes are minimal.


2015 ◽  
Vol 13 (1) ◽  
Author(s):  
Bozena Lozowicka ◽  
Ewa Rutkowska ◽  
Izabela Hrynko

AbstractLSE (liquid-solid extraction), MSPD (matrix solid phase dispersion) and QuEChERS (quick, easy, cheap, effective, rugged and safe) extractions followed by GC-μECD/NPD to determine 223 pesticide residues in tobacco simultaneously were developed and compared. The identities of ten model pesticides were confirmed by GC-MS/MS. The type and amount of dispersant (Florisil, silica gel and alumina), sample mass, cleanup adsorbent, and the eluent (hexane, acetone and acetonitrile) were optimized. Linearity, recovery, LOQ, LOD, and matrix effect were compared. Most recoveries were 71−120% (RSD < 18%). LOD and LOQ were much lower than the CORESTA GRLs. The best method was QuEChERS: acetonitrile extraction and dispersive solid-phase extraction using primary-secondary amine and graphitized carbon.


2020 ◽  
Vol 103 (1) ◽  
pp. 227-234 ◽  
Author(s):  
Mohammad Behbahani

Abstract Background: Because of trace amounts of atrazine in water samples and the complexity of the matrix, direct trace monitoring of atrazine is not feasible by the abovementioned techniques. Hence, an efficient sample pretreatment procedure is necessary for cleanup and preconcentration of atrazine from sample matrices. Objective: In the current paper, a new and efficient sample preparation method named solvent-assisted dispersive solid-phase extraction (SA-DSPE), followed by HPLC–UV, was introduced for the monitoring of atrazine at trace levels in environmental water samples. Methods: In the present method, benzophenone was used as a sorbent for extraction of target molecules. For dispersing solid sorbents in sample solution, very low milligram amounts of benzophenone and dispersive solvent were mixed and fast-injected into the extraction media. A cloudy solution formed, and after interaction of atrazine and the dispersed solid sorbent, the cloudy solution was centrifuged. The extracted atrazine in the solid phase was dissolved in ethanol and analyzed by HPLC–UV. Results: The introduced method showed a low method detection limit (0.1 μg/L), good precision (relative SD: 3.9–6.9%), and appropriate relative recoveries (95–105%). Conclusions: Within this study, a sensitive and reliable method for the quantification of atrazine in wastewater samples was successfully developed. Highlights: The obtained figures of merit for the presented sample preparation method were appropriate. The applicability of the method for analysis of atrazine in real matrices was excellent.


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