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A simple, green, rapid, and efficient ligandless dispersive liquid-liquid microextraction procedure based on solidification of a ternary deep eutectic solvent has been proposed for the extraction of trace amounts of Cd(II), Cu(II), and Pb(II) ions in milk samples prior to their determination by flame atomic absorption spectrometry. Initially, a suitable mole ratio of sorbitol, menthol, and mandelic acid are mixed in a test tube, and after heating, a deep eutectic solvent with low density compared to water is formed. The synthesized solvent is used as a chelating agent and an extraction solvent in the extraction of some heavy metal ions from milk samples. The influence of several effective parameters on the responses and extraction recoveries of the analytes was investigated. Under the optimum experimental conditions, the linear ranges were in the ranges of 1.0–40 μg L−1 for Cd(II) and Pb(II), and 1.0–25 μg L−1 for Cu(II). The obtained relative standard deviations (n = 6, C = 2.5 μg L−1 of each cation) and detection limits were in the ranges of 3.4–4.1% and 0.38–0.42 μg L−1, respectively. Finally, the developed method was successfully applied for the determination of Cd(II), Cu(II), and Pb(II) ions in different milk samples. Image 1 • An efficient ligandless DLLME method using a synthesized ternary DES is proposed for the extraction and preconcentration of Cd(II), Cu(II), and Pb(II) ions at trace levels from milk samples. • A few microliters of the synthesized DES was used simultaneously as a complexing agent and an extraction solvent, therefore, the extraction was performed without using any organic solvent. • This study is the first report on the application of the present method for the extraction of heavy metals in milk samples. • The proposed method offers numerous advantages, such as simplicity, ease of operation, and low cost. • The developed method was used for the determination of the analytes in different milk samples. [ABSTRACT FROM AUTHOR]

Abstract: In this study, a developed technique was reported for extraction and pre-concentration of methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) from urine samples using molecularly imprinted-solid phase extraction (MISPE) along with simultaneous derivatization and dispersive liquid–liquid microextraction (DLLME). Molecularly imprinted microspheres as sorbent in solid phase extraction (SPE) procedure were synthesized using precipitation polymerization with MAMP as the template. Aqueous solution of the target analytes was passed through MAMP-MIP cartridge and the adsorbed analytes were then eluted with methanol. The collected eluate was mixed with butylchloroformate which served as the derivatization reagent as well as the extraction solvent. The mixture was immediately injected into deionized water. After centrifugation, 1μL of the settled organic phase was injected into gas chromatography–flame ionization detection (GC–FID) or gas chromatography–mass spectrometry (GC–MS). Various experimental parameters affecting the performance of both of the steps (MISPE and DLLME) were thoroughly investigated. The calibration graphs were linear in the ranges of 10–1500ngmL−1 (MAMP) and 50–1500ngmL−1 (MDMA), and the detection limits (LODs) were 2 and 18ngmL−1, respectively. The relative standard deviations (%RSDs) obtained for six repeated experiments (100ngmL−1 of each drug) were 5.1% and 6.8% for MAMP and MDMA, respectively. The relative recoveries obtained for the analytes in human urine samples, spiked with different levels of each drug, were within the range of 80–88%. [Copyright &y& Elsevier]