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Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained., (Copyright © 2017 Elsevier B.V. All rights reserved.)

A simple sample pretreatment for simultaneous determination of nine fungicides (triadimefon, picoxystrobin, kresoxim-methyl, diniconazole, epoxiconazole, trifloxystrobin, triticonazole, difenoconazole, and azoxystrobin) in chrysanthemum was developed using matrix extraction-vortex-assisted dispersive liquid-liquid microextraction (ME-VADLLME) prior to gas chromatography with electron capture detection. The target fungicides were firstly extracted with acetonitrile and cleaned with the mixture of primary secondary amine and graphite carbon black. The VADLLME procedure was performed by using toluene with lower density than water as the extraction solvent and the acetonitrile extract as the dispersive solvent, respectively. After vortexing and centrifugation, the fine droplet of toluene was collected on the upper of the mixed toluene/acetonitrile/water system using a 0.1-mL pipettor. Under the optimum conditions, the relative recoveries ranged from 73.9 to 95.1% with relative standard deviations of 3.5-9.7% for all of the analytes. The limits of detection were in the range of (0.005-0.05)×10(-3) mg kg(-1). In the proposed method, the ME step provides more effective cleanup for the chrysanthemum matrix, and VADLLME introduces higher sensitivity with the remarkable enrichment factors up to 88-fold compared with the conventional QuEChERS or SPE. The good performance has demonstrated that ME-VADLLME has a strong potential for application in the multi-residue analysis of complex matrices., (Copyright © 2014 Elsevier B.V. All rights reserved.)

A novel analytical approach based on molecularly imprinted solid phase extraction (MISPE) coupled with dispersive liquid-liquid microextraction (DLLME), and injector port silylation (IPS) has been developed for the selective preconcentration, derivatization and analysis of 3-phenoxybenzoic acid (3-PBA) using gas chromatography-tandem mass spectrometry (GC-MS/MS) in complex biological samples such as rat blood and liver. Factors affecting the synthesis of MIP were evaluated and the best monomer and cross-linker were selected based on binding affinity studies. Various parameters of MISPE, DLLME and IPS were optimized for the selective preconcentration and derivatization of 3-PBA. The developed method offers a good linearity over the calibration range of 0.02-2.5ngmg(-1) and 7.5-2000ngmL(-1) for liver and blood respectively. Under optimized conditions, the recovery of 3-PBA in liver and blood samples were found to be in the range of 83-91%. The detection limit was found to be 0.0045ngmg(-1) and 1.82ngmL(-1) in liver and blood respectively. SRM transition of 271→227 and 271→197 has been selected as quantifier and qualifier transition for 3-PBA derivative. Intra and inter-day precision for five replicates in a day and for five, successive days was found to be less than 8%. The method developed was successfully applied to real samples, i.e. rat blood and tissue for quantitative evaluation of 3-PBA. The analytical approach developed is rapid, economic, simple, eco-friendly and possess immense utility for the analysis of analytes with polar functional groups in complex biological samples by GC-MS/MS., (Copyright © 2013 Elsevier B.V. All rights reserved.)