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BACKGROUND A combination of magnetic solid‐phase extraction using an efficient and cheap magnetic sorbent obtained from sand and dispersive liquid–liquid microextraction has been developed for the extraction of nine multiclass pesticides (clodinafop‐propargyl, haloxyfop‐R‐methyl, fenoxaprop‐P‐ethyl, oxadiazon, penconazole, diniconazole, chlorpyrifos, fenazaquin, and fenpropathrin) from commercial fruit juices (sour cherry, pomegranate, grape, watermelon, orange, apricot, and peach juices). The enriched pesticides were determined by gas chromatography–flame ionization detector and gas chromatography–mass spectrometry. The sorbent was natural iron oxide entrapped in silica along with some impurities. In this method, to extract the analytes from the samples, an appropriate amount of the magnetic sorbent (at mg level) is added. Then the sorbent particles are isolated from the solution using an external magnetic field and the adsorbed analytes are desorbed from the sorbent by acetone. In the following, a dispersive liquid–liquid microextraction procedure is carried out to concentrate the analytes more and to reach low limits of detection. RESULTS: Under optimized extraction conditions, the method revealed satisfactory repeatability (relative standard deviation ≤8% for intra‐day and inter‐day precision), reasonable extraction recovery (43.3–55.9%), high enrichment factors (433–559), and low limits of detection (0.45–0.89 μg L−1). CONCLUSION: The method was applied in the analysis of pesticides in various fruit juices. Chlorpyrifos was found in peach juice at a concentration of 27 ± 2 μg L−1 (n = 3) using a gas chromatography–flame ionization detector. To verify the results, the peach juice was also injected into gas chromatography–mass spectrometry after applying the proposed extraction method. © 2022 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

A vortex‐assisted dispersive micro‐solid‐phase extraction procedure using a new and green sorbent was developed as a simple, fast, and efficient sample preparation method for the extracting five pesticides in several fruit juice samples. In this study, for the first time, riboflavin was used as an efficient sorbent. A few milligrams of riboflavin was directly added into the aqueous solution containing the analytes to adsorb them. After adsorption the analytes, they were desorbed and more concentrated by a dispersive liquid–liquid microextraction procedure. The influence of several effective parameters such as amount of riboflavin, pH, vortex time, eluent nature and volume, and extraction solvent type and volume on the extraction efficiency was investigated. In optimal conditions, linear ranges of the calibration curves were broad. The limits of detection and quantification were attained in the ranges of 0.56–1.5 and 1.9–0.52 ng mL−1, respectively. The proposed method demonstrated to be suitable for concurrent extraction of the studied pesticides in various fruit juice samples with high enrichment factors (320–360) and precision (relative standard deviation ≤7.8% for intra‐ [n = 6] and interday [n = 4] precisions at a concentration of 25 ng mL−1 of each pesticide). [ABSTRACT FROM AUTHOR]

BACKGROUND: A method has been developed based on a three–phase system, followed by dispersive liquid–liquid microextraction for the extraction of seven pesticides from soya milk prior to analysis by gas chromatography‐flame ionization detection. The base of this method is the different extraction capability of the components of soya milk according to each of the phases involved. In this procedure, a homogeneous solution consisting of soya milk and a water–miscible solvent (acetonitrile) is separated into two phases in the presence of Na2SO4 and the analytes are extracted into the produced acetonitrile droplets. The acetonitrile phase is mixed with a pre‐concentration solvent to perform the next microextraction procedure for further enrichment of the analytes. RESULTS: Limits of detection and quantification were reached in the ranges of 0.11–0.35 and 0.35–1.20 µg L−1, respectively. Enrichment factors and extraction recoveries were in the ranges of 562–933 and 56–93%, respectively. Relative standard deviations were ≤7% for intra– (n = 6) and inter–day (n = 5) precisions at two concentrations of 10 and 50 µg L−1 of each analyte. CONCLUSION: The proposed method was applied to the analysis of pesticides in soya milk samples at µg L−1 concentrations. © 2019 Society of Chemical Industry [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]