scholarly journals SALLE combined with LD-DLLME for pesticides analysis in sugar and soil samples

2021 ◽  
Vol 35 (1) ◽  
pp. 1-16
Author(s):  
T. Tolcha ◽  
K. Gomoro ◽  
N. Megersa
Keyword(s):  
Pesticide Residues ◽  
Concentration Level ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Optimum Conditions ◽  
Salting Out ◽  
Liquid Liquid Extraction ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

In this study, a modified salting-out-assisted liquid-liquid extraction (SALLE) combined with low density dispersive liquid-liquid microextraction (LD-DLLME) has been developed for quantitative determination of multiclass pesticide residues (atrazine, diazinon, ametryn, terbutryn, chlorpyrifos, dimethametryn, 4,4'-dichlorodiphenyldichloroethylene (4,4'-DDE), 4,4'-dichlorodiphenyldichloroethane (4,4'-DDD) and 4,4'-dichloro- diphenyltrichloroethane (4,4'-DDT)) levels in sugar and soil samples coupled with gas chromatography–mass spectrometry (GC-MS) detection. The extract was enriched after combining SALLE to LD-DLLME and enrichment factor obtained ranged 30-121. Under the optimum conditions, the linearity of the method was in the range of 6.25–100 ng g-1 for atrazine, ametryn, terbutryn, dimethametryn and 4,4'-DDT, and in the range of 2.5–100 ng g-1 for diazinon, chlorpyrifos and 4,4'-DDD, and in the range of  1–100 for 4,4'-DDE with correlation coefficient of  0.992 or better. The limits of detection (LODs) ranged from 0.01–0.25 ng g-1. The precisions as %RSD, were below 10% for both matrices. The recoveries obtained from spiked sugar and soil samples at 5 and 50 ng g-1 ranged from 79 to 111%. The method was subsequently applied to real sugar and soil samples. All the pesticides investigated were not detected in the sugar sample. The soil sample was contaminated by atrazine and ametryn at concentration level of 0.3 and 0.2 ng g-1, respectively.                     KEY WORDS: SALLE, LD-DLLME, Extraction, Pesticide residues, Sugar, Soil   Bull. Chem. Soc. Ethiop. 2021, 35(1), 1-16. DOI: https://dx.doi.org/10.4314/bcse.v35i1.1  

Combination of Counter Current Salting-Out Homogenous Liquid–Liquid Extraction with Dispersive Liquid–Liquid Microextraction for the High-Performance Liquid Chromatographic Determination of Environmental Estrogens in Water Samples

2019 ◽  
Vol 58 (2) ◽  
pp. 171-177 ◽  
Author(s):  
Zhihong Shi ◽  
Qingru Huai ◽  
Xinye Li ◽  
Hongyu Ma ◽  
Can Zhou ◽  
...  
Keyword(s):  
Water Samples ◽  
High Performance ◽  
Liquid Extraction ◽  
Environmental Estrogens ◽  
Salting Out ◽  
Liquid Liquid Extraction ◽  
Dispersive Liquid Liquid Microextraction ◽  
Counter Current ◽  
Liquid Microextraction

Abstract In this paper, counter current salting-out homogenous liquid–liquid extraction was combined with dispersive liquid–liquid microextraction for the determination of environmental estrogens in water samples by high-performance liquid chromatography. In this method, initially, sodium chloride was filled into a syringe and a mixture of water sample and acetonitrile was driven to pass through the syringe. Due to salting-out effect, fine droplets of acetonitrile went up through the remaining mixture and aggregated as a separated layer on the top. Then, the collected organic phase (acetonitrile) was removed with a syringe and mixed with carbon tetrachloride (extraction solvent). In the second step, the mixed organic phase was rapidly injected into 5 mL of distilled water to further enrich the analytes. Good linearity was obtained in the concentration range of 2.0~200 ng/mL for diethylstilbestrol (DES) and 8.0~200 ng/mL for octylphenol (OP), respectively. Limits of detection were 0.09 ng/mL for DES and 0.20 ng/mL for OP, respectively. Relative standard deviations for intra- and inter-day precisions were less than 2.1 and 3.1%, respectively. Finally, the established method was successfully applied to determine DES and OP in river water, well water, bottled water and campus drinking water samples with recoveries in the range from 81.0 to 105.9%.

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