Development of an analytical method for pesticide residues in berries with dispersive solid phase extraction using multiwalled carbon nanotubes and primary secondary amine sorbents

2018 ◽  
Vol 10 (7) ◽  
pp. 757-766 ◽  
Author(s):  
Pengyue Zhao ◽  
Pedro J. J. Alvarez ◽  
Xuesheng Li ◽  
Canping Pan

A dispersive SPE with PSA and MWCNTs as sorbent material was developed for pesticide residue analysis in berry samples.

2018 ◽  
Vol 41 (12) ◽  
pp. 2613-2622 ◽  
Author(s):  
Javier González-Sálamo ◽  
Javier Hernández-Borges ◽  
María del Mar Afonso ◽  
Miguel Ángel Rodríguez-Delgado

2019 ◽  
Vol 2019 ◽  
pp. 1-10
Author(s):  
Tengfei Liu ◽  
Daifeng Yang ◽  
Jian Mao ◽  
Xueming Zhang ◽  
Minghui Dong

A simple, rapid, and reliable method based on dispersive solid-phase extraction (d-SPE) and gas chromatography-mass spectrometry (GC-MS) was developed for quantitating polychlorinated biphenyls (PCBs) in vegetable samples. Parameters affecting both the extraction yields and cleanup efficiency, including the type and volume of extraction solvent, extraction time, type and volume of cleanup sorbent, and cleanup time, were optimized. Matrix effects were evaluated, and matrix-matched calibration was recommended. Under the optimized conditions, carboxylated multiwalled carbon nanotubes (MWCNTs-COOH), which exhibit excellent adsorption capabilities due to large surface area and unique structure, were employed as d-SPE sorbent to remove interfering substances, rather than the analytes, from vegetable samples. Satisfactory linear relationship was observed for all PCBs across a concentration range of 5–500 μg/kg with correlation coefficients no less than 0.9993. Four representative vegetables (cucumber, tomato, lettuce, and cabbage) were selected as matrices for method validation. Each matrix was spiked at concentrations of 5, 10, and 100 μg/kg to evaluate recoveries, which ranged from 84.5% to 116.5% with relative standard deviations (n=6) between 0.6% and 17.6%. The limits of detection and the limits of quantification ranged from 0.3 to 1.4 μg/kg and 0.8 to 4.5 μg/kg, respectively. Twelve real vegetable samples were analyzed using the proposed method. Three of the target PCBs were detected in one lettuce sample with the total concentration of 17.9 μg/kg.


2020 ◽  
Vol 16 (4) ◽  
pp. 381-392
Author(s):  
Ayman A. Gouda ◽  
Ali H. Amin ◽  
Ibrahim S. Ali ◽  
Zakia Al Malah

Background: Cadmium (Cd2+) and lead (Pb2+) have acute and chronic effects on humans and other living organisms. In the present work, new, green and accurate dispersive micro solid-phase extraction (DμSPE) method for the separation and preconcentration of trace amounts of cadmium (Cd2+) and lead (Pb2+) ions in various food, water and tobacco samples collected from Saudi Arabia prior to its Flame Atomic Absorption Spectrometric (FAAS) determinations was developed. Methods: The proposed method was based on a combination of oxidized multiwalled carbon nanotubes (O-MWCNTs) with a new chelating agent 5-benzyl-4-[4-methoxybenzylideneamino)-4H- 1,2,4-triazole-3-thiol (BMBATT) to enrich and separate trace levels of Cd2+ and Pb2+. The effect of separation parameters was investigated. The validation of the proposed preconcentration procedure was performed using certified reference materials. Results: Analyte recovery values ranged from 95-102%, indicating that the method is highly accurate. Furthermore, precision was demonstrated by the relative standard deviation (RSD < 3.0%). The limits of detection were 0.08 and 0.1 μg L−1 for Cd2+ and Pb2+ ions, respectively. The preconcentration factor was 200. Conclusion: The proposed method was used for the estimation of Cd2+ and Pb2+ ion content in various real samples, and satisfactory results were obtained. The proposed method has high adsorption capacity, rapid adsorption equilibrium, extremely low LODs, high preconcentration factors and shortens the time of sample preparation in comparison to classical SPE.


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