scholarly journals Fast determination of phthalates in mussel samples by micro-matrix solid-phase dispersion (micro-MSPD) coupled with GC–MS/MS

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Nieves Carro ◽  
Ana Mouteira ◽  
Isabel García ◽  
María Ignacio ◽  
Julio Cobas

AbstractA fast, effective and low cost sample preparation method based on miniaturized matrix solid-phase dispersion (micro-MSPD) combined with gas chromatography coupled to tandem triple-quadrupole-mass spectrometry (GC–MS/MS) has been developed for the determination of six phthalate diesters (DMP, DEP, DBP, BzBP, DEHP and DnOP) in mussel samples. The six target compounds have been included in the list of priority pollutants by United States Environmental Protection Agency. The extraction step was optimized on real spiked mussel coming from Galician Rías by means of a factorial design. The final procedure involved the use of 0.45 g of sample, 0.5 g of dispersant agent (Florisil) and 3 mL of organic solvent (ethyl acetate). The optimized method was validated giving satisfactory analytical performance, low detection limits (0.09 to 6.73 ng g−1 dw) and high recoveries (93 and 114%). The validated method was applied to four real mussel samples coming from Galician Rías.

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.


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