Salting-out Assisted Liquid-Liquid Extraction for the Determination of Multiresidue Pesticides in Alcoholic Beverages by High Performance Liquid Chromatography

Abstract

Abstract:A salting-out assisted liquid-liquid extraction (SALLE) method followed by high-performance liquid chromatography with ultraviolet-visible detector (HPLC-UV/Vis) has been proposed for determination of five multiclass pesticides residues including, atrazine, ametryn, terbutryn, carbaryl and chlorothalonil from various alcoholic beverages: beer, wine and Ethiopian honey wine (Tej). Experimental parameters influencing the extraction efficiency of the method such as the type and concentration of salt, volume of acetonitrile (the extraction solvent) and pH of the sample were assayed and the optimum conditions were established. Under the optimum experimental conditions, matrix-matched calibration curves were constructed using beer sample as the representative matrix and good linearity over wide concentration ranges were obtained with coefficient of determination (r 2 ) of 0.997 or better. The limits of detection (LOD) and quantification (LOQ) of the method, which were determined as 3 and 10 times a signal-to-noise ratio (S/N), were in the ranges of 1.3-3.9 and 4.5-12.8 µg L -1 , respectively. Precisions studied in terms of repeatability and intermediate precision (with-in lab reproducibility) at two concentration levels have demonstrated acceptable %RSD values, which were less than 10% in both cases. The applicability of the method was also investigated by analyzing various alcoholic beverages and demonstrated satisfactory recoveries in the ranges of 71-104% with their corresponding %RSDs less than 10% in all cases. The results of the study revealed that the developed SALLE method is selective and efficient sample preparation procedure prior to quantitative analysis of the target analytes by HPLC-UV/Vis.

Salting-out assisted liquid–liquid extraction for the determination of ciprofloxacin residues in water samples by high performance liquid chromatography–diode array detector

“…For efficient extraction of ionizable and relatively polar compounds, pH of the sample solution plays a decisive role. The sample solution pH should be lower than the pK a of the analytes to obtain the target analytes in their unionized forms so that they have a higher tendency to partition into the organic phase [43]. The effect of varying pH values of the sample solution on the extraction efficiency was studied in the range of 3.0–8.0.…”

“…At acidic conditions they are in cationic form, which is important for their retention during the extraction. At basic conditions, the anionic species of both acidic and piperazinylic quinolones are less retained in comparison to cationic, zwitterionic and neutral species [43, 44].…”

A Review: Sample Preparation Methods for the Pesticide Residue Analysis in Food Samples

“…Salting out Liquid-Liquid extraction method followed by high performance liquid chromatography with ultraviolet-visible detector has been reported for the analysis of atrazine, ametryn, terbutryn, carbaryl and chlorothalonil in beer, wine and Ethiopian honey wine [3]. Under the optimum experimental conditions, matrix-matched calibration curves were constructed using beer sample as the representative matrix and good linearity over wide concentration ranges were obtained with R 2 of 0.997.…”

Copolymerized Natural Deep Eutectic Solvent Encapsulated in Calcium Alginate Beads: Application as a Green Sorbent for Analysis of Multiclass Pesticides in Nonalcoholic Malt Beverages by GC–MS/SIM

“…A literature survey revealed that a variety of sample preparation techniques based on liquid and solid phases within the years 2006−2021 had been published for the cleanup and extraction of pesticide residues in malt-based beverages, including solid-phase extraction (SPE), 14,15 solvent extraction (SE), 6,14,16,17 Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method, 7,13 liquid−liquid extraction (LLE), 18 and salting-out assisted LLE (SALLE) method. 19 These sample preparation methods have been coupled with gas chromatography−mass spectrometry selective-ion monitoring (GC−MS/SIM), 14 LC−MS/MS, 13,15,16,18,20 gas chromatography−electron capture detection (GC−ECD), 17 gas chromatography−mass spectrometry (GC−MS), 18 gas chromatography with tandem mass spectrometry (GC−MS/MS), 7 and liquid chromatography with ultraviolet/visible. 19 The aim of this work was to develop a green analytical procedure for the analysis of multiclass pesticide residues in nonalcoholic malt beverages.…”

“…19 These sample preparation methods have been coupled with gas chromatography−mass spectrometry selective-ion monitoring (GC−MS/SIM), 14 LC−MS/MS, 13,15,16,18,20 gas chromatography−electron capture detection (GC−ECD), 17 gas chromatography−mass spectrometry (GC−MS), 18 gas chromatography with tandem mass spectrometry (GC−MS/MS), 7 and liquid chromatography with ultraviolet/visible. 19 The aim of this work was to develop a green analytical procedure for the analysis of multiclass pesticide residues in nonalcoholic malt beverages. For this, a green alternative micro-solid phase extraction based on natural materials was developed.…”